Polymer Synthesis - Science topic

By the way, it is not fully clear whether it is a copolymerization or grafting. This later is achieved by attaching a chemical/motif to an already formed polymer, is it your situation ?

Hello Saya Bird,

the purification depends on the polymer and the side products/impurities, which you want to remove.

Additional purification methods might be following:

Dialysis; I used this to remove some salts, which could leave the polymer solution through the membrane of the dialysis tube, whereas the polymer remained in the tube.

Fractionated precipitation: I used this to separate blockcopolymers from homopolymers or different moecular weight fractions of the same polymer from each other. You add a non solvent to a polymer solution and the less soluble polymer (depending on their chemistry in the case of block copolymer) or the polymer with the higher molecular weight (in the case of different molecular weights) precipitates first as a polymer gel.

There are also methods, that require more elaborate equipment, like preparative GPC or separation by LCCC.

If your separation does not remove the impurities, maybe add the solvent slower (drop by drop, as you mentioned) and use another solvent (or non-solvent). Maybe you polymer precipitates so easily, that the impurities are trapped in your solid polymer. If the polymer precipitates slower the impurities may stay dissolved (similar to the case of fractionated precipitation).

The confirmation of your product also depends on the polymer. Maybe some groups on your monomer were changed by the polymerization, which could be detected by IR-spectroscopy.

For the chracterization of polyurethanes (as an example), remaining isocyanate groups can be titrated.

If you use a new method to obtain a known polymer, you can also compare it's properties with literature values (i.e. the glass transition temperature via DSC) to get a hint if the reaction might have worked.

There are plenty of complex and simple methods to characterize a polymer, but it depends on your polymer if you can use them.

It will depend upon the degree of unsaturation in the monomeric units, concentration of it and strength of oxidizing agent.

Except the analyses that have been mentioned, you can performe ATR-FTIR analysis to determine its chemical stucture.

Dear Yuewen Jia, whatever the color is, it should be purified by sublimation prior to its use. My Regards

Dear Cole Carpenter, I would like to put the following remarks. The amount of MAC is to be taken in slight excess with the equivalent number of OH end groups and not with respect to the PEO MW. The same thing to pyridine, with respect to the presumed evolved amount of HCl. There are many reviews dealing with the end functionalization of PEGs and PEOs end groups, an example is in the following RG thread I posted years ago. My Regards

Raja Summe Ullah

Yes, it is possible. check von Braun degradation.

May be the ReaxFF bond boost method could also be useful?

See also this tutorial: https://www.scm.com/doc/Tutorials/MolecularDynamicsAndMonteCarlo/PolymersBondBoost.html

Dear Mohamed Chaala, the best is the one that insures high solvation and low transfer reaction. The solvent is much more choosen with respect to the monomer first. My Regards

Irgacure-2959

Respected Professor,

I am Dr. Chiragkumar M. Patel, presently working as a research associate supervised by Dr. KVSN Raju, at Division of Polymers & Functional Materials, Indian Institute of Chemical Technology Hyderabad. It’s my ardent interest to enhance my research aptitude by further exploring the challenges in the field of polymer science coupled with sustainable chemistry.

My current research work is schemed involving the methodology of non isocyanate polyurethane coatings for high performance functional materials.

My doctoral thesis was headed as - “Synthesis and characterization of polyol from agriculture waste and its applications”. My work during the tenure of Ph.D. included systematic preparation, characterization and applications of prepared bio-based polymeric precursor. My research was just not confined to the above work but has a wider extension, leading to application of rigid polyurethane, adhesives as well as in the field of smart two-pack coating system whose outcome will be reflected in my upcoming publications.

My laboratory virtues are:

Maturity, honesty, trouble shooting and the ability to deal with challenges as great opportunities. An enthusiast and hardworking researcher in a highly interdisciplinary and collaborative environment. Volunteer responsibility with a cheerful countenance and pursues task diligently. Ability to work in group and lead a team. My research interests include sustainable chemistry by synthesizing bio-based polymeric precursor and characterization, looking into their application towards polyurethane based coating, adhesives and rigid foam and finally study of their mechanical and chemical properties. My C.V., is attached to this mail for your kind consideration.

Thank you and looking forward to hearing from you soon.

With best regards,

Sincerely yours,

Dear Xin Li, following are interesting documents. My Regards

Dear Ramish Riaz, if kinetics consistency is important then you have to repeat the synthesis with respect to the reference procedure. You did not said any thing about evolved water elimination! Reversibility of the reaction by hydrolysis may occurs before restarting. My Regards

Dear all, the problem is related to the electrospinning process parameters and not due to the polymer itself. Please check these documents. My Regards

DOI: 10.5772/53459

Dear all, what is the role of sonication in your case? Is it for mixing/dispersion or for reaction assisting. If it is for the later option you can use microwaves. My Regards

Dear all, you can not use AIBN or any type of radical initiator. Your monomers are not vinylic or acrylic. If it is a ring oppening polymerization ionic initiation is more suitable, though in some special cases radical initiators may work. My Regards

I agree Jing Jin, You can try to change the solvent of emulsion polymerization because that the content of 1.3 butadiene is controlled by the polarity of the solvent.

Abdelkader BOUAZIZ @ Thanks alot,,

Dear Mariam,

Can you please give me the details of your polymer and the solvent suitable for dissolution? I might be able to perform few experiments for you.

I think you should use stronger bases as catalysts like organic superbases. Often guanidines are good catalysts for aza-Michael addition, like tetramethylguanidine or TBC (triazabicyclo decene). But also P4-tBu, a phosphazene base should work. DBU and DABCO are a little bit worse in such reactions but better than normal trialkylamines. It should work in neat at temperatures below 100°C.

You have an additional problem, the complete incompatiblity of the two reactants. This problem can be overcome by addition of a polyether modified polysilicon. Such products are sold from byk as defoamers or air release additives : https://www.byk.com/en/additives/product-groups/defoamers-air-release-additives.html

Perhaps also a non-ionic emulsifier helps, like tween 80.

Hi,

Please see the above link:

https://chemeng.queensu.ca/people/Faculty/AndrewDaugulis/files/2013/Eduardo_JCTB_2014.pdf.

With my best regards

I think there are a few options for you to try. I'm assuming your compound is symmetric, but if it wasn't and depending on the size, you could use HMBC to confirm covalent bonds (or lack thereof). I'm guessing this isn't an option though.

¹H NMR you might be able to see a hydroxyl peak and you might even see new peaks appear (very close to 0) instead of a single peak, as the electronic environment where the ring opened will be slightly different. These shifts are very small so I can't guarantee you'd see clearly resolved peaks. Also note that these shifts may appear below 0 ppm.

IR would also show a broad and diagnostic OH peak if the ring opened, which would be very quick and easy to assess. This would be the first thing I would try.

In theory, you would see a different mass on MS but I don't think these would fly well (likely be destroyed by ionization).

Finally, I would say TLC could potentially be used as you'll see a new spot with a much lower Rf. Ceric Ammonium Molybdate (CAM) should stain very strongly for hydroxyl groups; you could also try stains that give different colors (e.g., vanillin and p-anisaldehyde), as I expect the silanol group would give rise to a very different color. This wouldn't give you a conclusive answer, but it might give you enough of a clue to feel confident.

If exhausting this arsenal of characterization techniques gives you only equivocal results of whether or not your ring opened, then I would suggest going to ²⁹Si NMR. If your institute has easy access to these more exotic NMR nuclei then this should be a good way to get a definitive answer.

Hi;

I suggest you read the following patent: WO2014131747A1 (Novel method for purifying polyesters).

With my best regards

I would take hydrazine hydrate. But I could imagine more efficient procedures. Iron (III) is extracted form aqueous acidic solutions in chloroform with tributylphophine oxide as ligand. It could be suffient to treat an acidic suspension of PEDOT with tributylphosphineoxide and extract the iron in chloroform. Also dioctylarsinic acid can be used as ligand to achieve extraction in organic media.

Hi Ponambala,

It may be due to high foaming or due to improper reaction....

Dear Alam,

this rule particularly concerns the diols used for production of polyesters exploited in the textile industry. Monomeric units derived from linear-alpha,omega-diols namely allow linear supramolecular arragement of macromolecules and thus formation of crystallites giving to fibres high axial tensile strength. However, if one consider applications in the field of coatings, also polyols with branched chains are useful and used.

I agree with you

I agree with Karol, however the solubility will depend on the HPMA/MMA ratio as well as on the final molecular weight of copolymer.

While flash chromatography is a viable method for small quantities, I have used activated granular carbon to remove the MEHQ. The carbon was 4-8 mesh (large granular for easy handling) that was placed in a vacuum drying oven at 120C for 24 hours. This was then added to the acrylate to adsorb the MEHQ. The slurry was gently mechanically agitated for good mixing. Please use a mechanical agitator, not a magnetic spin bar (as the bar tends to 'grind' the carbon to smaller powder against the bottom of the beaker/pot). You can monitor the MEHQ content, adding additional carbon and agitation time until you reach the desired inhibitor content. Then simply filter the carbon off of the acrylate. If you totally deplete all of the inhibitor, use the monomer as soon as possible. Acrylic acid polymerization is self accelerating (giving off a lot of heat of polymerization) and can result in a violent (read explosive) reaction (conditions).

I recommend removal of inhibitor on only amounts you can use within 24 hours of filtering. So long as the monomer is in contact with the carbon-MEHQ, I have not had any stability problems. Once filtered, the monomer is VERY reactive.

I have used this method with a number of different acrylate and methacrylate monomers, with sizes of 100 grams up to 10 kilos in an industrial setting.

the catalysts may vary upon choice of materials or precursors we used. you can choose your favorable compunds. there are 1000s of studies reported with different catalysts. its hard to find review on all available catalyst. i have compiled articles which repoted various catalyst. i will mail you the articles.

all the best

Yes, For distilling dioxan I recommended what Anup Kumar mentioned, using chromatographic grade basic Al2O3 to remove impurities including peroxides and reflux it for several hours over sodium wire and distilled under nitrogen or argon and stored in the dark.

Hi Tanzeel, this is a while after your experiment, but would you be able to give the concentration of PLGA and PEG you used for your synthesis? I'm running into a similar problem myself so it'd be very helpful to hear what ratios/concentrations you used. Thanks!

The most important solvents for melamine are: water, DMSO and

polyhydroxyl alcohols in which it has the highest solubility of 2-5.7 g in

diols and of 10.0 g in glycerol in 100 g of solvent, at 140°C

or this ref:

Kucharski M., Głowacz-Czerwonka D.: Solubilization of nitrogen-containing heterocyclic compounds in reactive solvents. J. Appl. Polym. Sci. 2002, 84 (14), 2650.

Głowacz-Czerwonka D., Kucharski M.: New melamine–formaldehyde–ketone polymers. II. Dissolution of melamine in reactive solvents prepared from cyclohexanone. J. Appl. Polym. Sci. 2005, 96 (1), 775.

Głowacz-Czerwonka D., Kucharski M.: New melamine–formaldehyde–

ketone polymers. V. Coatings from melamine and MEK-based reactive solvents.J. Appl. Polym. Sci. 2008, 109 (4), 2156.

In Origin, you can set the axes length of X:Y =1 by going to the layer section of graph in size/speed section

1% could be 1% by volume or 1% by mass. This is not defined.

If we get to 100 mL of final solution then (by volume) 1 mL of PVA needs to be diluted in 99 mL of water (to make 100 mL total - Lewis's final concentration is 1/101 and thus not 1% w/v...). However, if there's volume change then this isn't the most appropriate way - here the comment of Rafik is applicable (dissolve 1 mL or 1 g in 50 mL and make up to 100 mL in a standard flask)

Hi,

In-situ photopolymerization is very robust method to obtain polymer nanocomposites. It is eco-friendly (solvent free process) and also facile way for fabricating especially membranes and thin films. Furthermore, it provides a number of advantages, e.g. homogeneity and time, compared to thermal process (either shaping or reaction).

Best regards.

yes you can do it, you need another monomer that has an attractor group to synthesize a copolymer to improve performance

Thank you everyone. I am using this monomer (3,3'-Dihydroxybenzidine). it contains two primary amine groups. polymerization involves Monomer like this, they used NMP as solvent. what is the advantage using NMP over DMAc.

last time i synthesized aminated polyaryl ether sulfone. But tyhe molecular weight was low.

(ODA) Surfactant.a treatment with an epoxy resin-functionel grop by (ODA) Surfactant. a treatment with an epoxy resin-functionel grop by (ODA) Surfactant.you can useing a treatment with an epoxy resin-functionel grop by (ODA) Surfactant.

Thank you very much for sharing these papers

Dear Angel,

you shoud try of vacuum shouk method . I think it might help.In addition It would be great rather fast - avoiding long-term swelling .

see can you Publication : Effect of bubble based degradation on the physical properties of Single Wall Carbon Nanotube/Epoxy Resin composite and new approach in bubbles reduction Article Aug 2016 · Composites Part A Applied Science and Manufacturing Seyyed Alireza Hashemi · Seyyed Mojtaba Mousavi

Good luck with your research!

To see if PCL-diol polymer has film-forming properties, there is any easy method:

You need to have a metallic ring "the size of a small hand bracelet" which contains little mercury placed inside a glass dish. Pour the polymer's solution over mercury & let the solvent evaporate without heating in a fume cupboard. After that, try to take the film by means of tweezers. If you cannot pull a circular film & you see that it has crumbled, then the polymer does not have fiber-forming properties. Conversely, a film formed is indicative of success, of course.

One source of methods is to consider searching commercial patents especially US ones - have done this for PCM in the past and found them useful if you have some knowledge to start with.

Thank You 

Thank you sir, for your kind response to my enquiry. Can you please send any published article related to this.

Dear Samaneh salkhi, I advise you that, add an excess of BD as the terminating agent after the molecular weight reached into 4000. The alpha hydroxy group of lactic acid will react slow compared to HO of BD. The unreacted or excess of BD will be removed in hexane solvent.   

Bio-absorbable Polymers in Implantation-An Overview, J Scientific & Industrial Research, 68 (2009) 993-1009.

Fluorescence-detectable, star-shaped polylactic acid construction for implantation. European Polymer Journal. 48 (2012) 1357–1360.

Dear Julia,

I haven't worked with pullulan or dextrans but I was working with starch carboxymethylation, where isopropanol is also good solvent for etheryfication.

1. Isopropanol is good precipitating medium for starch (starch granules slightly swells but gelatinization is avoided) and final product of carboxymethylation for the one hand and isopropanol is good solvent for other reagents (like monochloroacetic acid).  This solvent is also good precipitation medium for the other polysaccharides with lower molecular weight.

2. Acctually the best solvents for nucleophilic substitutions S_N2 are aprotic media (you can look at here: http://www.sciencedirect.com/science/article/pii/0144861795000836), but starch reguires polar media for alkalization (first step of etherification) St-OH + NaOH  --> St-O^- Na⁺ + H₂O. So some extra water affect reaction efficiency.

3. It can be related to screening effect and relative polarity of organic solvent (isop. has lower relative polarity than methanol or ethanol). Properties of the solvent influences on occuring or efficiency of side reactions (sodium glycolates).  

 http://onlinelibrary.wiley.com/doi/10.1002/star.200300239/epdf

4. Even if reaction is conducted in organic solvent excess of NaOH leads to home decrease in aver. molecular weight of polysaccharide chains.

 https://www.researchgate.net/profile/Magdalena_Zdanowicz/publication/262377037_Carboxymethyl_starch_with_high_degree_of_substitution_Synthesis_properties_and_application/links/02e7e5377f47cc2e49000000.pdf

Meybe attached articles will be helpful anyway.

Best regards

Thank you all!

According to use chain transfer agent to control molecular weight, how to decide the amount of CTA should be added? early experience or reference would be appreciated!

Poly(acrylamide-co- diallyldimethylammonium chloride) -see the structure in the file below- will most probably meet your requirements. The copolymer Poly (AAm-co-DADMAC) is definitely water-soluble & my expectation is that it is EtOH-insoluble.

Since the polymer contains ionic bonds plus extra strong secondary bonds, its melting point is expected to be very high.

Needless to say that it doesn't  have any hydroxy, carboxylic, and amine functional groups in the side chain. There are amide & ammonium yes but they differ from the 3 mentioned functional groups.

However, experimentation with a small amount of polymer or copolymer can give better information than anything else.  

 I agree fully with Dr. BOUAZIZ.  Chain transfer reactions cause PDI to get much larger than 2 (as is common especially with many polyolefin materials).

The explanations given in an earlier answer, about stoichiometric imbalance, will get you PDI < 2 (rather  than PDI > 2).  Also, crosslinking is not really relevant for polycarbonates which is a thermoplastic.

There are no methods of soft chemistry. There are methods for synthesizing a soft mutter. Examples of soft substances: surfactant micelles, proteins, enzymes, supramolecular substances .... Solvents are involved in the organization of the volumetric form of these substances. Their shape, volume affects the temperature, pressure, solvents, inorganic electrolytes. Some of them are prepared by polymerization. They are usually water-soluble high-molecular compounds polyethylene oxide, polyacrylamide. When the conditions change, they form globules in the water. Globules combine and form gels.Therefore, they differ from a solid mutter.

Thanks Mrinmay Mandal, i tested the solubility PCL in acetone. DCM, DMF, chlorofrom and THF ( Mw of PCl = 65k-80k). DMF and THF cannot dissolve PCL. 

I mean that when I created the literature review about this, Some papers give incorrect information, maybe not clear. I need some informative and reliable papers which related to this topic

This is a patent for phenothiazine removal

Also, look at previous question, I'm almost certain this has come up in the past.

CHPO as the oxidant , and thiourea derivatives & triethyl amine as the reducing agents in the formulation system.

wash in very dilute ammonia will react the excess and crosslink then wash in water = alternatively dilute alkaline material

As mentioned above, Grubbs  3 is one of the fastest catalyst. It's unlikely you will get the same results as for the Grubbs catalysts of the 1st generation that were used in the paper. My guess is that all monomer is consumed before you have all components properly mixed, resulting in unreacted catalyst and catalyst wit nobornene oligomers attached. You could try to decrease the reaction temeperature or use more equivalents of monomer. We did similar experiments with Grubbs 3 and got a full initiation with 5 equiv. of a modified norbornene. Furthermore, make sure that you really have unreacted catalyst, as the propagating species appears in NMR as two resonances / double peak (cis and trans).See attached figure and links.

By oxidation with different oxidants. The main problem is the control of the oxidation reaction.

Dear all,

chemical titration of the double bond is a simple way. Small aliquots are taken along the course of polymerization and rapidly quenshed in cold hydroquinone solution to stop any further polymerization after sampling. Here I suppose it is a polyaddition polymerization and not a step-growth one. Regards

Your question falls apart into 2 parts: 1. Making paraformaldehyde (PF) solutions, 2. Measuring molecular weight (MW).

1. Literature suggests that dimethylsulfoxide (DMSO) is suitable as a solvent for PF, provided that temperature is not too high. See attached file (Johnson et al., 1975).

2. Measuring MW by intrinsic viscosity is only feasible if results can be compared with at least 2 standard PF samples with known MW, which may be problematic. Moreover, MW of PF seems to be rather low, with degrees of polymerization ranging from 8-100 according to Wikipedia. Such low values could also make the use of osmotic pressure and light scattering problematic. Perhaps the best way is to use freezing point depression (FPD) in DMSO, because this quantity only depends on the number of molecules in solution and not on solute type. So you can compare FPD of your sample with FPD of e.g. sucrose, preferably at a range of concentrations. If you have sensitive NMR equipment available, you could also try to estimate MW from the amount of terminal H or C. Please note that DMSO is hygroscopic.     

For aliphatic diisocyanates, like HDI, IPDI (often the best candidate of aliphatic diisocyanates), hydrogenated MDI or TMXDI the best catalyst is DBTL which can be applied in amounts of  200-1000 ppm. Tin dilaurate, Desmorapid SO, is the best catalyst for aromatic diisocyanates like TDI or MDI. Bismuth neodecanoate can be used for all isocyanates in amounts of at least 1000 ppm but has the advantage that it is less sensitive against water, because it catalyses the reaction of isocyanate and alcohol faster than the reaction between isocyanate and water. For better dosage the catalyst can be thinned in THF as already explained by Jatin Sethi. High amounts of catalysts have no negative influence on the polyaddition reaction itself but on the stability of the resulting polyurethane. DMSO and NMP are not optimal in PU formation because they are not "innocent" solvents. They can also react with the diisocyanate. They should only be applied if the diol component is not soluble in other solvents. THF is in most cases the best solvent for PU reaction, but also MEK - and if the solubility of the diol allows it - halogenated hydrocarbons, esters or aromatic solvents are appropriate. The concentration of reactants and polymer can be in the range of 25 %. The stoichiometry should be near 1:1. In several cases a slight isocyanate excess of 1% could be advantageously. Dryness of the diol and the solvent is crucial for a good urethane formation, because water destroys isocyanate under CO2 evolution (Bi catalyst better than Sn in respect to the water reaction but less active). 

Phenol-formaldehyde resins, which are obtained from phenols and formaldehyde, have the greatest practical importance. Depending on the relative amounts of the reactants and the nature of the catalyst, the reaction produces either novolacs or resols resins. Thus, in the presence of acid catalysts (usually hydrochloric or oxalic acid) and an excess of phenol, novolac resins are obtained; in the presence of basic catalysts, such as NaOH, Ba(OH)2, and NH4OH, and an excess of formaldehyde, resols are formed.

Their color depends on the type of catalyst used in production and ranges from light yellow to reddish. However, do not forget the effect of phenol and phenol type as well. Phenol-formaldehyde resins harden during processing upon heating; with novolac resins, however, a hardener is required (usually hexamethyl-enetetramine). In addition, synthesize, curing, time, temperature can also affect the color.

Hope this will help. 

Parhalad Sharma

Please, clarify your question !  

Have you added thionyl chloride to the lactone and you ended up with polymer !!!?

Good luck

Combustion of PVDF produces hydrogen fluoride

I'd recommend recirculating the melted polyester in a single screw or double screw extruder.  The heat (Tm +20) and shearing action of the extruder will gradually break down the molecular weight through beta-scission and autooxidation--if antioxidants are present, they will eventually be consumed. By converting screw torque into viscosity values, you can estimate the rate of molecular weight degradation.  As Florian said above, a little moisture will accelerate MW degradation by ester hydrolysis. You may be able to do your reactive copolymerization directly in the extruder if it will dissolve into the melt.

Dear Rahul,

Distil aniline with a water steam - it forms hetero-azeotrop containing 19,2 % of aniline that boils at 98.7 °C. Aniline containing dissolved water is obtained from distillate by decantation since it forms sepaprate phase.     For polymerization, you do not need to dry so obtained aniline, because polymerization is carried out in aqueous environment. You only take into account that, at 25 °C, equilibrium content of water in aniline is 4,76 weight % !

Best regards, J.V.

many thanks dears Abdelkader BOUAZIZ and Navneet Kumar

You can try using emulsion polymerization in water medium. It would avoid using solvent, but you have to do experiments if incorporating uv curable additives possible. Good luck!

A viscometer (also called viscosimeter) is an instrument used to measure the viscosity of a fluid. For liquids with viscosities which vary with flow conditions, an instrument called a rheometer is used. Thus, a viscometer can be considered as a special type of rheometer. Viscometers only measure under one flow condition.

Standard laboratory viscometers for liquids

-U-tube viscometers

-Falling sphere viscometers

-Falling ball viscometer

-Falling piston viscometer

-Oscillating piston viscometer

-Vibrational viscometers

-Quartz viscometer

-Rotational viscometers

-Electromagnetically spinning sphere viscometer (EMS viscometer)

-Bubble viscometer

-Rectangular-slit viscometer

As you mentioned, your Polyurethane are gel samples and resulted of the reaction of MDI with Lignin isolates. I think the viscosity of your samples are quite high, you might need to use the right equipment and accessories for the measurement. Some rotational viscometers with the right selection can help you to do so.

Good luck!

Dear Dr. Tsanov,

Thank you so much for your answer. Could you send me the method you used?

Beste regards

Petrus

The reactivity of a simple alkoxide is too low to effectively initiate anionic polymerisation of styrene. Thus, if you obtain a polymer at all, you will loose control on molar mass and on dispersity (due to slow initiation) .

 There might be some Special systems, which might be able to inititate styrene polymerisation. But these are certainly not simple alkoxides but will require additional additives/coinitiators etc.

What exactly is C5?

Normally the peroxide curing of EPDM is done in neat with a peroxide of high decomposition temperature (e.g. dicumylperoxide) at 160-180°C. It is not usual to do it in solution. If you use a solution the chain transfer constant of the solvent is crucial. Toluene exhibit a relative high chain transfer so that most of the radicals are consumed by abstracting hydrogen from the methyl group of the toluene. Benzene is the best solvent in respect to low chain transfer followed by chlorobenzene. With these solvents you will have a better chance. Mostly a co-curing reagent is added to peroxide curing of EPDM like TMP-trimethacrylate, triallylisocyanurate, triallylcyanurate or bismaleinimides from MDA or TDA. These co-curing reagents will further increase the chance to get a gel.

But if you have already a solution of EPDM you can also epoxidize its double bonds (in the easiest cse) with m-chloroperbenzoic acid. The epoxidized EPDM can be easily crosslinked with amines like isophorone diamine (IPDA). This peroxide free procedure will work in every case and is easier in the laboratory than radical vulcanization. 

I am assuming that the number you have is in meq/g (see for instance: http://www.huntsman.com/performance_products/Media%20Library/a_MC348531CFA3EA9A2E040EBCD2B6B7B06/Products_MC348531D0B9FA9A2E040EBCD2B6B7B06/Amines_MC348531D0BECA9A2E040EBCD2B6B7B06/Polyetheramines%20%20%20JE_MC348531D0E07A9A2E040EBCD2B6B7B06/Diamine%20products_MC348531D0EA1A9A2E040EBCD2B6B7B06/files/JEFFAMINE%20D-2000_US.pdf). Then there is ca. 330 g/eq. However, for epoxy reactions, there are two reactive groups so the epoxy based equivalent weight is half that. For curing with isocyanates, you can assume 1 reactive group (the second is usually neglected). Thus the equivalent weight is 330 g/eq or 165 g/eq. From this information alone you cannot determine functionality.

I would suggest to dissolve the polymer in toluene and wash by shaking in a separating funnel with diluted HCl.

You can mesure the solid content, by putting the sample of the emulsion in a convection oven at 120°C for 4h. If the monomers are polymerized they contribute to the solid, otherwise they evaporate together with the water. In the case of quantitative conversion you will find all monomers as polymer in the solid content.

yes I agree, you can take into account extra modification with fibers of different ypes: natural like Rami and synthetic.

Janik