CN102746506A - Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization - Google Patents
Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization Download PDFInfo
- Publication number
- CN102746506A CN102746506A CN2012102083090A CN201210208309A CN102746506A CN 102746506 A CN102746506 A CN 102746506A CN 2012102083090 A CN2012102083090 A CN 2012102083090A CN 201210208309 A CN201210208309 A CN 201210208309A CN 102746506 A CN102746506 A CN 102746506A
- Authority
- CN
- China
- Prior art keywords
- chlorohydrin rubber
- homopolymerization
- precipitation polymerization
- parts
- homopolymerization chlorohydrin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Abstract
The invention discloses a method for preparing homopolymerization chlorhydrin rubber by deposition polymerization. The method comprises a step of mixing 10 to 70 parts by volume of a low-polarity organic solvent, 5 to 16 parts by volume of an epichlorohydrin and 1 to 5 parts by volume of a catalyst, a step of reacting for 1 to 5 hours at a temperature of 50 to 80 DEG C, and a step of separating and purifying to obtain the homopolymerization chlorhydrin rubber The preparation technology provided by the invention is simple in method and low in cost, and the prepared product has beautiful appearance, excellent mechanical properties and strong practicality.
Description
Technical field
The invention belongs to the chlorohydrin rubber field, be meant that specifically a kind of precipitation polymerization prepares the method for homopolymerization chlorohydrin rubber.
Background technology
Homopolymerization type chlorohydrin rubber is the viton by the epoxy chloropropane ring-opening polymerization, is a kind of oil resistant, heat-resisting and specialty elastomer that ventilation property is very low.The oil-proofness of homopolymerization type chlorohydrin rubber, especially anti-halogenated alkane performance surpasses paracril; Thermotolerance between paracril and acrylic elastomer, heat-resisting 150 ℃ of short-term, long-term heat-resisting 100 ℃; Ventilation property is lower than butyl rubber.Homopolymerization type chlorohydrin rubber is mainly used in the various oil resistant sealing members of system, barrier film, tackiness agent and freon resistant sebific duct etc.Because it is do not have two keys in the chlorohydrin rubber molecular chain, so its heat-proof aging is good with ozone resistance,, warping strength, elasticity is all good again because of there being the ehter bond of easy internal rotation.Characteristics such as side group chlorine atom provides oil resistant, anti-solvent, anti-burning, ventilation property is low, binding property is good, so over-all properties is superior to paracril and X 050, price is lower than viton and Zylox.Chlorohydrin rubber is the very wide product of a kind of application prospect, has excellent performance.All be widely used in automotive industry, refrigerator industry, power industry, petroleum industry, chemical fertilizer industry, space industry and electronic industry.
Chlorohydrin rubber is realized suitability for industrialized production in nineteen sixty-five by U.S. He Gelisi company and Gu Te Ritchie chemical company, and then Nippon Zeon Co., Ltd. also begins to produce, but produces the national few of chlorohydrin rubber, and output is also lower.At present, the preparation method of domestic chlorohydrin rubber mainly is solution with toluene, carries out solution polymerization and produces chlorohydrin rubber.The chlorohydrin rubber of producing like this is no matter be the aspects such as outward appearance, mechanical property at product, or the production cost of chlorohydrin rubber etc. is not ideal.
Summary of the invention
The objective of the invention is the method and the product that provide a kind of precipitation polymerization to prepare the homopolymerization chlorohydrin rubber according to above-mentioned deficiency, with the homopolymerization chlorohydrin rubber of this method preparation excellent mechanical not only, and outward appearance is beautiful, and is with low cost.
The present invention realizes through following technical scheme: a kind of precipitation polymerization prepares the method for homopolymerization chlorohydrin rubber; Its step comprises: with volume parts is that the low polar organic solvent of 10-70 part, epoxy chloropropane and the volume parts that volume parts is 5-16 part are the catalyst mix of 1-5 part; Can obtain said homopolymerization chlorohydrin rubber in reaction under 50-80 ℃ after the separation and purification after 1-5 hour.
Said low polar organic solvent is a kind of in sherwood oil, normal heptane, normal hexane or the hexanaphthene.
Said being reflected under the nitrogen atmosphere carried out.
Preferably, said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 80-100:160-200:12-25.
Most preferred, said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 100:200:16.
After said separation and purification was meant the decompress filter solvent, drying under reduced pressure obtained said homopolymerization chlorohydrin rubber under 50-60 ℃ of temperature.
Homopolymerization chlorohydrin rubber provided by the invention is to adopt precipitation polymerization reaction of the present invention to obtain, and when having solved domestic employing solution polymerization process and preparing the homopolymerization chlorohydrin rubber, bubble is too much in the chlorohydrin rubber product, product mechanical property problem of lower.And need solvent distillation during prior art production homopolymerization chlorohydrin rubber, energy consumption is big, so production cost is higher; Preparation technology's method of the present invention is simple; The product appearance for preparing is beautiful, and only suction filtration can obtain the homopolymerization chlorohydrin rubber, therefore saves cost; And excellent mechanical has very strong practicality.
Description of drawings
Fig. 1 is the infrared spectrogram of homopolymerization chlorohydrin rubber 1;
Embodiment
Below further specify the present invention through specific embodiment:
With volume parts is the catalyst mix that 65 parts sherwood oil, epoxy chloropropane that volume parts is 15 parts and volume parts are 3 parts; Under nitrogen atmosphere; Stop reacting by heating in reaction under 70 ℃ after 3 hours, after the logical cold water cooling; The vacuum filtration solvent gets elastomerics, and obtains little yellow to shallow white granular homopolymerization chlorohydrin rubber 1 in 50 ℃ of following vacuum-dryings.Said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 100:200:16.The limiting viscosity of homopolymerization chlorohydrin rubber 1 [η] is 0.2734; The viscosity-average molecular weight M of product
ηBe 114726.
Embodiment 2
With volume parts is the catalyst mix that 10 parts normal heptane, epoxy chloropropane that volume parts is 5 parts and volume parts are 1 part; Under nitrogen atmosphere; Stop reacting by heating in reaction under 50 ℃ after 1 hour, after the logical cold water cooling; The vacuum filtration solvent gets elastomerics, and obtains little yellow to shallow white granular homopolymerization chlorohydrin rubber 2 in 55 ℃ of following vacuum-dryings.Said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 80:200:25.
Embodiment 3
With volume parts is the catalyst mix that 70 parts normal hexane, epoxy chloropropane that volume parts is 16 parts and volume parts are 5 parts; Under nitrogen atmosphere; Stop reacting by heating in reaction under 80 ℃ after 5 hours, after the logical cold water cooling; The vacuum filtration solvent gets elastomerics, and obtains little yellow to shallow white granular homopolymerization chlorohydrin rubber 3 in 60 ℃ of following vacuum-dryings.Said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 100:160:12.
Embodiment 4
With volume parts is the catalyst mix that 65 parts hexanaphthene, epoxy chloropropane that volume parts is 15 parts and volume parts are 3 parts; Under nitrogen atmosphere; Stop reacting by heating in reaction under 70 ℃ after 3 hours, after the logical cold water cooling; The vacuum filtration solvent gets elastomerics, and obtains little yellow to shallow white granular homopolymerization chlorohydrin rubber 4 in 50 ℃ of following vacuum-dryings.Said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 90:180:16.
As shown in Figure 1, absorption frequency is 744.27cm
-1The time, peak value is obvious, and the stretching vibration that has C-Cl key is described.Absorption frequency is at 1100 cm
-1When neighbouring, peak value is strong, and the stretching vibration that has O-C-O key is described.Absorption frequency is near 1500cm
-1The time, more small peak appears, existence-CH is described
2Flexural vibration with-CH-middle C-H key.Absorption frequency is at 2875.06 cm
-1With 2900.78 cm
-1Shi Youfeng explains existence-CH
2Stretching vibration.
Chlorohydrin rubber is shredded after mixing, be put in the dumbbell shaped mould, be placed on then on the thermocompressor, temperature is transferred to 155 ℃, heating 15min under 10MPa, heating 10min under 20MPa heats 30min at last under 30MPa then.The rubber black in color, softness, elasticity is little.
The homopolymerization chlorohydrin rubber 1 that vulcanizates is carried out tensile test at microcomputer control electronics universal testing machine (CMT6503); The tensile strength of this sintetics is 0.62MPa, obviously is superior to the product (identical cure conditions stretched intensity is 0.49MPa) of domestic solution polymerization.
Claims (6)
1. a precipitation polymerization prepares the method for homopolymerization chlorohydrin rubber; Its step comprises: with volume parts is that the low polar organic solvent of 10-70 part, epoxy chloropropane and the volume parts that volume parts is 5-16 part are the catalyst mix of 1-5 part; Can obtain said homopolymerization chlorohydrin rubber in reaction under 50-80 ℃ after the separation and purification after 1-5 hour.
2. prepare the method for homopolymerization chlorohydrin rubber according to the said precipitation polymerization of claim 1, it is characterized in that: said low polar organic solvent is a kind of in sherwood oil, normal heptane, normal hexane or the hexanaphthene.
3. prepare the method for homopolymerization chlorohydrin rubber according to the said precipitation polymerization of claim 1, it is characterized in that: said being reflected under the nitrogen atmosphere carried out.
4. prepare the method for homopolymerization chlorohydrin rubber according to the said precipitation polymerization of claim 1, it is characterized in that: said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 80-100:160-200:12-25.
5. prepare the method for homopolymerization chlorohydrin rubber according to the said precipitation polymerization of claim 4, it is characterized in that: said catalyzer is triisobutyl aluminium, phosphoric acid and N, the accelerine of volume ratio 100:200:16.
6. prepare the method for homopolymerization chlorohydrin rubber according to the said precipitation polymerization of claim 1, it is characterized in that: after said separation and purification was meant the decompress filter solvent, drying under reduced pressure obtained said homopolymerization chlorohydrin rubber under 50-60 ℃ of temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102083090A CN102746506A (en) | 2012-08-07 | 2012-08-07 | Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102083090A CN102746506A (en) | 2012-08-07 | 2012-08-07 | Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102746506A true CN102746506A (en) | 2012-10-24 |
Family
ID=47027029
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012102083090A Pending CN102746506A (en) | 2012-08-07 | 2012-08-07 | Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102746506A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351466A (en) * | 2013-06-13 | 2013-10-16 | 江汉大学 | Method for preparing unsaturated terpolymer polyepichlorohydrin rubber through precipitation polymerization |
| CN107787342A (en) * | 2015-04-27 | 2018-03-09 | 密执安州立大学董事会 | Durability dredges ice surface |
-
2012
- 2012-08-07 CN CN2012102083090A patent/CN102746506A/en active Pending
Non-Patent Citations (3)
| Title |
|---|
| 《化学通报》 19771231 湖北省化学研究所 合成氯醇橡胶催化剂--三异丁基铝-磷酸-叔胺催化体系 第20-21页 1-6 , 第3期 * |
| 湖北省化学研究所: "合成氯醇橡胶催化剂——三异丁基铝-磷酸-叔胺催化体系", 《化学通报》 * |
| 湖北省化学研究所: "合成氯醇橡胶的高效催化剂", 《化学通报》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351466A (en) * | 2013-06-13 | 2013-10-16 | 江汉大学 | Method for preparing unsaturated terpolymer polyepichlorohydrin rubber through precipitation polymerization |
| CN107787342A (en) * | 2015-04-27 | 2018-03-09 | 密执安州立大学董事会 | Durability dredges ice surface |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103232598B (en) | Plant oil benzoxazine copolymer elastomer preparation method | |
| CN113248675A (en) | Cardanol-based self-repairing shape memory polymer and preparation method and application thereof | |
| CN106280488A (en) | A kind of silicone rubber of compression set function admirable and preparation method thereof | |
| CN105062085A (en) | Addition-type organosilicone mould rubber and preparation method thereof | |
| CN111471297B (en) | Preparation method and application of bio-based transparent polyamide | |
| CN102746506A (en) | Method for preparing homopolymerization chlorhydrin rubber by deposition polymerization | |
| CN106554481A (en) | A kind of method of In-sltu reinforcement epoxy resin | |
| CN106220922A (en) | Dynamic vulcanization polypropylene flame redardant/nitrile rubber thermoplastic elastomer and preparation method thereof | |
| CN110183852A (en) | A kind of tear-proof silicon compounded rubber stock and preparation method thereof | |
| CN102731767A (en) | Method for preparing copolymer chlorohydrin rubber by precipitation polymerization | |
| CN113698593A (en) | Composite material and preparation method thereof | |
| CN107189196B (en) | A kind of polypropylene material and preparation method thereof of low smell environment-friendly type | |
| CN114149586B (en) | Chain-extended polysulfate and preparation method thereof | |
| CN111073018B (en) | PBT/fluorine film composite film and production process thereof | |
| CN103665381A (en) | Synthesis method of hydroxyl capped polydimethylsiloxane | |
| CN103351466A (en) | Method for preparing unsaturated terpolymer polyepichlorohydrin rubber through precipitation polymerization | |
| CN103755962A (en) | Production method for high-vinyl raw rubber | |
| WO2018129779A1 (en) | Polyolefin thermoplastic elastomer and processing method therefor | |
| CN114940808B (en) | Recyclable epoxy resin Vitrimer material and preparation method thereof | |
| CN115304745B (en) | Resveratrol and isovanillin based bio-based composite epoxy resin and preparation method thereof | |
| CN110591082B (en) | Copolymerized nylon resin and preparation method and application thereof | |
| CN108659452A (en) | A kind of preparation method of heat safe air conditioning for automobiles flabellum | |
| CN103965236B (en) | A kind of polycarbonate chainextender and preparation method thereof | |
| CN116554534B (en) | Environment-friendly polypropylene flame-retardant foam material and preparation process thereof | |
| CN101456956B (en) | CN group-containing organosilane co-polymer modified cyanate ester resin and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20121024 |