CN104045753A - Polyvinyl dichloride (PVDC) composition for carbon molecular sieve - Google Patents
Polyvinyl dichloride (PVDC) composition for carbon molecular sieve Download PDFInfo
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Abstract
The invention discloses a polyvinyl dichloride (PVDC) composition for a carbon molecular sieve. The PVDC composition comprises the following components in parts by weight: 160-165 parts of deionized water, 0.07-0.35 part of dispersing agent, 0.2-0.5 part of initiator, 0.04-0.25 part of pH buffer regulator, 70-100 parts of vinylidene chloride monomer and 0.05-0.25 part of nano filler. The PVDC composition has the advantage of good product performance.
Description
Technical field
The present invention relates to a kind of PVDC composition, in particular, the present invention relates to a kind of carbonaceous molecular sieve PVDC composition.
Background technology
Polyvinylidene dichloride (PVDC) is the homopolymer of vinylidene chloride (VDC) or taking vinylidene chloride as main component and the polymkeric substance that forms of other monomer copolymerization.Due to the existence of symmetrical structure and the hydrophobic group chlorine of molecular chain, PVDC has higher crystallinity and fusing point, blocks water, oxygen resistance is good, and the barrier of gas is not subject to the impact of ambient moisture, is widely used in the fields such as chemical industry, light industry, packaging, food.
Apparent density and porous body product are large, fusing point is high, volatile content is low, the PVDC that three order concentration ratios are high passes through high pressure pressing mold, high temperature pyrolysis produces the porous ungraphitised carbon with highly cross-linked structure, aperture can reach nano level, close with molecular dimension, can make Powdered, pearl, the different shape such as block or discoid, powder, pearl can be worked as filler, bulk or disk stack in placing container and use, there is the general characteristic of common carbonaceous molecular sieve, and the high gas storage of density space is large, intensity is high, wear and tear low, conduction and thermal conductivity are high, selectivity is high, it is a kind of carbon structure of high-quality of porous.PVDC after high pressure pressing mold or high temperature pyrolysis can be used for adsorbing multiple gas-liquid, and separating high-purity gas processed aspect with normal temperature low pressure aspect the safety in transportation and storage of the high-risk gas (hydrogen arsenide, phosphuret-(t)ed hydrogen, boron trifluoride etc.) using in the time of semiconductor microelectronics manufacturing processed intermediate ion implanting device has good application.
The synthetic of PVDC carried out to a large amount of research both at home and abroad, but it is less for the synthetic method report of the PVDC composition of gas adsorption to be applicable to being made into PVDC carbonaceous molecular sieve.As China Patent Publication No. CN103408688A, November 27 2013 publication date, denomination of invention: a kind of preparation method of PVDC composition.This application case has been introduced a kind of preparation method of PVDC composition, by composition of raw materials, 54～56% deionized water, the pH value dash adjustment agent aqueous solution, 20～80% mix monomer, 20～80% initiator, 20～80% aqueous dispersant are joined in polymeric kettle, cold dispersion is after 30 minutes, under 40～100rpm mixing speed, be warmed up to 65～80 DEG C and start polyreaction, simultaneously add remaining reaction raw materials with friction-motion speed, added and stopped polyreaction after rear continuation polyreaction 2～4h and obtain PVDC composition.Weak point is that apparent density and the porous body product of the PVDC composition that makes is less, is not suitable for being made into PVDC carbonaceous molecular sieve for gas adsorption, has limited the Application Areas of PVDC composition.
Summary of the invention
The present invention is directed to the deficiencies in the prior art part, the carbonaceous molecular sieve that a kind of product performance are good PVDC composition is provided.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is: a kind of carbonaceous molecular sieve PVDC composition, and by weight, it is composed as follows:
As the preferred embodiment of the present invention, described carbonaceous molecular sieve PVDC composition, by weight, also comprises the comonomer of 2～20 parts.
As the preferred embodiment of the present invention, described pH dash adjustment agent is preferably one or more the mixture in Sodium Acid Pyrophosphate, Sodium phosphate dibasic, trisodium phosphate, sodium bicarbonate, ammonium acetate.
As the preferred embodiment of the present invention, described initiator is preferably the one in peroxy dicarbonate ethylhexyl, di-isopropyl peroxydicarbonate, new peroxide tert-butyl caprate, 2,2'-Azobis(2,4-dimethylvaleronitrile), dilauroyl peroxide, dibenzoyl peroxide, the special butyl ester of peroxidation-2 ethyl hexanoic acid.
As the preferred embodiment of the present invention, described dispersion agent is preferably the one in methylcellulose gum, Vltra tears, methyl cellulose ether.
As the preferred embodiment of the present invention, described nano-filled material is preferably the one in nano silicon, nano-calcium carbonate, nano titanium oxide.
As the preferred embodiment of the present invention, described comonomer is preferably the one in vinylchlorid (VC), methyl methacrylate (MMA), vinyl cyanide (AN).
The present invention is by optimizing PVDC composite formula, the index such as fusing point, apparent density, fugitive constituent, three order concentration ratios of having improved PVDC composition, carbonaceous molecular sieve of the present invention stores the carbonaceous molecular sieve making that separates high-purity gas use processed with normal temperature low pressure by PVDC composition particularly suitable gas adsorption.The PVDC composition fusing point that the present invention makes is greater than 195 DEG C, and apparent density is at 0.6～0.8g/cm
3.
Fusing point of the present invention refers to the corresponding temperature of composition thermal absorption enthalpy maximum value, and its measuring method can adopt the ordinary method of this area as dsc (DSC) mensuration.Carbonaceous molecular sieve of the present invention is measured by cup type method by the apparent density of PVDC composition, gravimetric determination in baking oven for fugitive constituent.
The agent of PH dash adjustment can make the pH value of polymerization system be difficult for changing, PH dash adjustment agent in the present invention is preferably one or more the mixture in Sodium Acid Pyrophosphate, Sodium phosphate dibasic, trisodium phosphate, sodium bicarbonate, ammonium acetate, and its parts by weight are 0.04～0.25 part.
Initiator is heated and can decomposes generation free radical, to cause chain polymerization, initiator in the present invention is preferably the one in peroxy dicarbonate ethylhexyl, di-isopropyl peroxydicarbonate, new peroxide tert-butyl caprate, 2,2'-Azobis(2,4-dimethylvaleronitrile), dilauroyl peroxide, dibenzoyl peroxide, the special butyl ester of peroxidation-2 ethyl hexanoic acid, and its parts by weight are 0.2～0.5 part.
Dispersion agent can be adsorbed in liquid-solid interface and can significantly reduce interfacial free energy, pressed powder is dispersed in liquid or melt uniformly, and makes it not reassociate.Dispersion agent in the present invention is preferably the one in methylcellulose gum, Vltra tears, methyl cellulose ether, and its parts by weight are 0.07～0.35 part.
Nano-filled material is mainly used in material surface processing, can improve dispersiveness and the resin bonding of material, nano-filled material in the present invention is preferably the one in nano silicon, nano-calcium carbonate, nano titanium oxide, and its parts by weight are 0.05～0.25 part.
Comonomer mainly improves the processing characteristics of PVDC composition, comonomer in the present invention is preferably the one in vinylchlorid (VC), methyl methacrylate (MMA), vinyl cyanide (AN), and its parts by weight are 2～20 parts.
Compared with prior art: the present invention has following beneficial effect:
1, fill a prescription by aggregation, the index such as fusing point, apparent density, fugitive constituent, three order concentration ratios of having improved PVDC composition, carbonaceous molecular sieve of the present invention stores the carbonaceous molecular sieve making that separates high-purity gas use processed with normal temperature low pressure by PVDC composition particularly suitable gas adsorption;
2, product performance are good, and the PVDC composition fusing point that the present invention makes is greater than 195 DEG C, apparent density 0.66g/cm
3above, fugitive constituent is below 0.16%, and three order concentration ratios (60 orders, 80 orders, 100 orders) are more than 90.25%, are specially adapted to make carbonaceous molecular sieve.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail, but the present invention is not only confined to following examples.
The particular product performance parameters that embodiment and comparative example make adopts following methods to measure:
Fusing point adopts dsc (DSC) to measure;
Apparent density is measured by cup type method;
Gravimetric determination in baking oven for fugitive constituent;
Resin screening is pressed GB/T20022 standard and is carried out, and three order concentration ratios (60 orders, 80 orders, 100 orders) account for the ratio of gross weight for falling into the weight in this three orders interval.
Example 1
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation process is as follows:
(1) ready reaction raw material for standby, reaction raw materials consists of:
(2) the preparation pH dash adjustment agent aqueous solution and aqueous dispersant: by trisodium phosphate 1.6kg and Sodium phosphate dibasic 0.4kg, deionized water 20kg is mixed with the pH dash adjustment agent aqueous solution; By methyl cellulose ether 2.5kg, deionized water 375kg is mixed with aqueous dispersant;
(3) the preparation of nano stopping composition aqueous solution: by 1.8kg nano silicon, 88.2kg deionized water is mixed with the nano-filled material aqueous solution;
(4) 257.3kg deionized water, the pH dash adjustment agent aqueous solution are joined to 3M
3polymeric kettle (band whipping appts stainless steel polymeric kettle, length-to-diameter ratio is 2:1, three leaf anchor formula oars) in, after the pressure testing of envelope still, use nitrogen replacement 3 times, after vacuumizing, add VDC monomer, initiator (peroxy dicarbonate ethylhexyl), after stirring and mixing for 15 minutes, add aqueous dispersant and the nano-filled material aqueous solution, add remaining deionized water.Cold dispersion, after 30 minutes, to the logical hot water of jacket of polymerization, is warmed up to 65 DEG C and starts polyreaction under 70rpm mixing speed, increase mixing speed with 5.6rpm/h speed simultaneously, polyreaction 8h stops polyreaction, and vacuum is deviate from residual monomer, is cooled to 45 DEG C of dischargings, centrifugal, dry.
Result: the white resin making, have good stability, 195 DEG C of fusing points, apparent density 0.77g/cm
3, fugitive constituent 0.15%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.69%.
Example 2
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, have good stability, and 198 DEG C of fusing points, apparent density 0.72g/cm
3, fugitive constituent 0.14%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 91.54%.
Example 3:
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, have good stability, and 198 DEG C of fusing points, apparent density 0.69g/cm
3, fugitive constituent 0.14%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.72%.
Example 4
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 201 DEG C of fusing points, apparent density 0.75g/cm
3, fugitive constituent 0.15%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 91.14%.
Example 5
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 198 DEG C of fusing points, apparent density 0.78g/cm
3, fugitive constituent 0.16%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 91.65%.
Example 6
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 202 DEG C of fusing points, apparent density 0.74g/cm
3, fugitive constituent 0.13%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 91.42%.。
Example 7
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 197 DEG C of fusing points, apparent density 0.72g/cm
3, fugitive constituent 0.16%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.65%.
Example 8
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 200 DEG C of fusing points, apparent density 0.73g/cm
3, fugitive constituent 0.14%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.56%.。
Example 9
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 199 DEG C of fusing points, apparent density 0.71g/cm
3, fugitive constituent 0.16%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.67%.
Example 10
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 197 DEG C of fusing points, apparent density 0.66g/cm
3, fugitive constituent 0.13%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.37%.
Example 11
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 196 DEG C of fusing points, apparent density 0.68g/cm
3, fugitive constituent 0.14%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 90.25%.
Example 12
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is better, 198 DEG C of fusing points, apparent density 0.71g/cm
3, fugitive constituent 0.16%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 91.46%.
Comparative example 1
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, stability is general, 168 DEG C of fusing points, apparent density 0.62g/cm
3, fugitive constituent 0.45%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 85.14%.
Comparative example 2
A kind of carbonaceous molecular sieve PVDC composition, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, less stable, 160 DEG C of fusing points, apparent density 0.55g/cm
3, fugitive constituent 0.65%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 86.14%.
Comparative example 3:
A preparation method for PVDC composition for carbonaceous molecular sieve, its composition of raw materials is as follows:
Preparation method is with embodiment 1, result: the white resin making, less stable, 174 DEG C of fusing points, apparent density 0.65g/cm
3, fugitive constituent 0.36%, three order concentration ratio (60 orders, 80 orders, 100 orders) is 84.31%.
Claims (7)
1. a carbonaceous molecular sieve PVDC composition, is characterized in that by weight, it is composed as follows:
2. carbonaceous molecular sieve according to claim 1 PVDC composition, is characterized in that by weight, also comprises the comonomer of 2～20 parts.
3. the preparation method of PVDC composition for carbonaceous molecular sieve according to claim 1 and 2, is characterized in that described pH dash adjustment agent is one or more the mixture in Sodium Acid Pyrophosphate, Sodium phosphate dibasic, trisodium phosphate, sodium bicarbonate, ammonium acetate.
4. the preparation method of PVDC composition for carbonaceous molecular sieve according to claim 1 and 2, is characterized in that described initiator is the one in peroxy dicarbonate ethylhexyl, di-isopropyl peroxydicarbonate, new peroxide tert-butyl caprate, 2,2'-Azobis(2,4-dimethylvaleronitrile), dilauroyl peroxide, dibenzoyl peroxide, the special butyl ester of peroxidation-2 ethyl hexanoic acid.
5. the preparation method of PVDC composition for carbonaceous molecular sieve according to claim 1 and 2, is characterized in that described dispersion agent is the one in methylcellulose gum, Vltra tears, methyl cellulose ether.
6. the preparation method of PVDC composition for carbonaceous molecular sieve according to claim 1 and 2, is characterized in that described nano-filled material is the one in nano silicon, nano-calcium carbonate, nano titanium oxide.
7. the preparation method of PVDC composition for carbonaceous molecular sieve according to claim 2, is characterized in that described comonomer is the one in vinylchlorid, methyl methacrylate, vinyl cyanide.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105131169A (en) * | 2015-08-14 | 2015-12-09 | 湖州新奥利吸附材料有限公司 | Carbon molecular sieve PVDC composition |
| CN106794443A (en) * | 2014-06-30 | 2017-05-31 | 陶氏环球技术有限责任公司 | Carbon molecular sieve adsorbing composition and its method based on vinylidene chloride copolymer |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174304A (en) * | 1981-04-20 | 1982-10-27 | Nippon Zeon Co Ltd | Production of electroconductive vinyl chloride resin composition |
| CN101580563A (en) * | 2009-05-21 | 2009-11-18 | 浙江巨化股份有限公司电化厂 | Preparation method of PVDC composition by VDC/MA copolymerization |
| CN103408688A (en) * | 2013-07-16 | 2013-11-27 | 浙江衢州巨塑化工有限公司 | Preparation method of PVDC composition |
-
2014
- 2014-06-19 CN CN201410276116.8A patent/CN104045753A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS57174304A (en) * | 1981-04-20 | 1982-10-27 | Nippon Zeon Co Ltd | Production of electroconductive vinyl chloride resin composition |
| CN101580563A (en) * | 2009-05-21 | 2009-11-18 | 浙江巨化股份有限公司电化厂 | Preparation method of PVDC composition by VDC/MA copolymerization |
| CN103408688A (en) * | 2013-07-16 | 2013-11-27 | 浙江衢州巨塑化工有限公司 | Preparation method of PVDC composition |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106794443A (en) * | 2014-06-30 | 2017-05-31 | 陶氏环球技术有限责任公司 | Carbon molecular sieve adsorbing composition and its method based on vinylidene chloride copolymer |
| CN106794443B (en) * | 2014-06-30 | 2020-03-27 | 陶氏环球技术有限责任公司 | Carbon molecular sieve adsorption composition based on vinylidene chloride copolymer and method thereof |
| CN105131169A (en) * | 2015-08-14 | 2015-12-09 | 湖州新奥利吸附材料有限公司 | Carbon molecular sieve PVDC composition |
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