CN1125735A - Synethsis method of pentadiene graft copolymer - Google Patents
Synethsis method of pentadiene graft copolymer Download PDFInfo
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- CN1125735A CN1125735A CN 94114277 CN94114277A CN1125735A CN 1125735 A CN1125735 A CN 1125735A CN 94114277 CN94114277 CN 94114277 CN 94114277 A CN94114277 A CN 94114277A CN 1125735 A CN1125735 A CN 1125735A
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- pentadiene
- graft copolymers
- temperature
- oxidation inhibitor
- polymkeric substance
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Abstract
The process for synthesizing pentadiene graft copolymer that features low cost, better low-temp properties, thermal stebility and dynamic or static sealing performance, and high slipping nature includes such steps as polymerization of pentadiene copolymer, E/VAC polymer, rosin powder and coupling agent, mixing the polymer with strengthening agent and antioxidant at 40-160 deg.C for 5-15 min, and low-temp granulating.
Description
The present invention relates to a kind of graft copolymers synthetic method, especially a kind of pentadiene graft copolymers synthetic method that is applied to the preserving and sealing field.
At present, this product in chemical industry aspect novel material application preserving and sealing field still belongs to blank in China.This novel material belongs to China's oil and natural gas line is badly in need of material, all be from external import, and have only the West Germany and the U.S. that similar graft copolymers is arranged abroad, and be to be base-material with vinylbenzene, butylbenzene, its synthetic graft copolymers poor performance at low temperatures (can only be in minimum temperature-40 ℃, use temperature is low more just immalleable), poor heat stability can only reach 260 ℃, slip property is low, and the import price costliness.
The objective of the invention is to overcome the deficiency of above-mentioned prior art, a kind of low-temperature performance is good, thermal stability is good, intensity is high, slip property is good and provide, the synthetic method of the similar graft copolymers of energy import substitution.
Purpose of the present invention can reach by following measure: the pentadiene copolymer of fusing and E/VAC polymkeric substance, colophonium powder, coupling agent carry out polyreaction, then with polymkeric substance and strengthening agent, that oxidation inhibitor together adds kneading device is mixing.
Purpose of the present invention can also reach by following measure: the consumption proportion of pentadiene copolymer, E/VAC polymkeric substance, colophonium powder, strengthening agent, oxidation inhibitor, coupling agent is respectively 30-38%, 4-10%, 20-32%, 25-36%, 0.8-2%, 0.2-1.4%.The pentadiene copolymer temperature of fusion is 110 ℃-160 ℃, and the time is 10-40 minute; Polymeric reaction temperature is 120 ℃-155 ℃, and the time is 3-20 minute; Melting temperature is 40 ℃-100 ℃, and the time is 5-15 minute.Strengthening agent is titanium dioxide and light calcium carbonate mixture, and the two content ratio is 1: 3; Coupling agent is vinyl three (β-oxyethyl group) silane.Oxidation inhibitor is 1010 oxidation inhibitor and the attached aid anti-oxidants of LDTP.
The present invention compares with existing technology has following positively effect: (1) is basic raw material owing to having adopted pentadiene copolymer and E/VAC polymkeric substance, has replaced external vinylbenzene, butylbenzene raw material, and cost is reduced; (2) be raw material owing to having taked pentadiene copolymer and E/VAC polymkeric substance, taked suitable temperature, pressure and additive to make the graft copolymers low-temperature performance good, still have good toughness and intensity in the time of-70 ℃; (3) excellent heat stability, decomposition temperature can reach 300 ℃; (4) slip property height has good dynamic and static sealing property.Be the synthetic graft copolymers performance index of pentadiene below: 85-152 ℃ of heat decomposition temperature 250-307 ℃ of project indicator melt index 10-15g/10min proportion 1.1-1.15g/cm3 Vicat softening point
(existing import connect the skill thing be 260 ℃) loss on heating (180 ℃)＜1.5% embrittlement temperature＜-70 ℃
(existing import connect the skill thing for＜-40 ℃) shearing resistance normal temperature-10＞1.0MPa
(it is 0.8MPa that existing import connects the skill thing) stripping strength (190 ℃) 30PaS erosion resistance (soaking 7d)
10%HCL shearing resistance＞1.0MPa
10%NaCL shearing resistance＞1.0MPa
10%Na (OH) shearing resistance＞1.0MPa describes the present invention in detail below in conjunction with synthesis process flow diagram:
Pentadiene copolymer is melted before connecing the skill reaction, its controlled temperature is 110 ℃-160 ℃, fusing time 10-40 minute, to heat gradually, the raw material that fusing is good is put the polymerization stirring tank into and is made it to stir with E/VAC polymkeric substance, colophonium powder, coupling agent and make the three fully carry out polyreaction.Controlled temperature is 120-155 ℃, and the time is 3-20 minute, puts it into the kneading device of heating then, and puts into strengthening agent and oxidation inhibitor, makes it fully plasticizing and modification, and melting temperature is 40-100 ℃.Dividing three sections carries out, (the emphasis here was the tensile strength that solves material in time 5-15 minute, antioxidant property, technical indicators such as thermostability and chemical stability), be that the examination and test of products, metering packing, finished product are dispatched from the factory at last after cryogenic freezing granulation process (5 ℃-20 ℃ freezing).The pentadiene graft copolymers, it is the very strong synthetic graft copolymers of a kind of bounding force, be mainly used in the anticorrosion and boats and ships of steel pipe composite structure, rot-resistant middle layer, metallic surface binding, its outstanding feature is a kind of graft copolymers that has two kinds of functions concurrently, dynamic seal after promptly static adhesive seal and the slippage.Pentadiene is synthetic to connect the agent multipolymer, and it has, and polarity is strong, force of cohesion big, the characteristics of high viscosity, but also has dynamic seal and static seal after the extraordinary slippage, makes anti-corrosion pipeline improve three times work-ing life.For the operation of the long-term safety of pipeline provides good condition, increase economic efficiency.
The pentadiene graft copolymers with regard to sticking intensity, all has good cementability and sealing persistence with surfaces such as steel, epoxy powder or lacquer, plastics, polyethylene, rubber.
Pentadiene synthesizes graft copolymers, and excellent mechanical property is also arranged, shock-resistant anti tear, anti-bending, withstand voltage and good elasticity and workability energy arranged.Better chemical and thermostability are arranged.(its heat decomposition temperature can reach more than 300 ℃) and not embrittlement of low temperature, low temperature resistant is-70 ℃, this is any rubber, the inaccessible performance of plastic or other material, also has good electrical insulation properties and the cracking performance of anti-the environmental stress.Product is convenient to store and transportation, uses reprocessing easily.Provide several embodiment below, further specify the present invention.
Embodiment one prescription:
1, pentadiene copolymer (IIR) 38%
2, the E/VAC polymkeric substance 10%
3, colophonium powder 32%
4, titanium white+light calcium carbonate 36%
TiO2 CaCO3 1∶3
5, antioxidant 1010 and LDTP 2%
6, coupling agent A172 1.4% method:
1, pentadiene copolymer is pulverized the back and carry out 40 fractional meltings by 160 ℃ at melting appartus.
2, melt is added polymerization reaction kettle, add E/VAC polymkeric substance, colophonium powder, coupling agent simultaneously, gather reaction, temperature is decided to be 155 ℃, 20 minutes time.
3, after the polyreaction material being added kneading device, to carry out low temperature mixing, adds antioxidant 1010 and LDTP, titanium dioxide+light calcium carbonate simultaneously, and melting temperature is 100 ℃, mixing time 11 minutes.
4, after fully mixing material is discharged bar shaped or sheet shape, carry out cryogenic freezing-10 ℃, carry out pelletizing again and be finished product.
Embodiment two prescriptions:
1, pentadiene copolymer (IIR) 30%
2, the E/VAC polymkeric substance 4%
3, colophonium powder 20%
4, titanium white+light calcium carbonate is 1: 3 25%
5, antioxidant 1010 LDTP 0.8%
6, coupling agent A172 0.2% method:
1, pentadiene copolymer is pulverized the back 110 ℃ of melting appartus temperature, fusing time 10 minutes.
2, melt is added polymerization reaction kettle, add E/VAC polymkeric substance, colophonium powder, coupling agent simultaneously and carry out polyreaction, temperature is 120 ℃, 5 minutes time.
3, after the polyreaction, material is added kneading device, and to carry out low temperature mixing, adds oxidation inhibitor, strengthening agent simultaneously, and temperature is 40 ℃, 8 minutes time.
4, after mixing material is caused bar shaped or sheet, carry out low temperature-18 and ℃ carry out granulation.Embodiment three prescriptions:
1, pentadiene copolymer (IIR) 34%
2, the E/VAC polymkeric substance 6%
3, colophonium powder 28%
4, strengthening agent 30%
5, antioxidant 1010 LDTP 1.2%
6, coupling agent A172 0.8% method:
1, the pentadiene copolymer temperature of fusion is 110 ℃, 20 minutes time.
2, melt is added polymerization reaction kettle, add E/VAC polymkeric substance, colophonium powder, coupling agent simultaneously and carry out polyreaction, temperature is 140 ℃, 5 minutes time.
3, after the polyreaction, material is added kneading device, and to carry out low temperature mixing, adds oxidation inhibitor, strengthening agent simultaneously, and temperature is 46 ℃, 8 minutes time.
4, after mixing material is caused bar shaped or sheet, carry out low temperature-5 and ℃ carry out granulation.
Claims (5)
1, a kind of pentadiene graft copolymers synthetic method is characterized in that the pentadiene copolymer and E/VAC polymkeric substance, colophonium powder, the coupling agent that melt carry out polyreaction, then with polymkeric substance and strengthening agent, that oxidation inhibitor together adds kneading device is mixing.
2, according to the described a kind of pentadiene graft polymerization thing synthetic method of claim 1, it is characterized in that the consumption proportion of pentadiene copolymer, E/VAC polymkeric substance, colophonium powder, strengthening agent, oxidation inhibitor, coupling agent is respectively 30-38%, 4-10%, 20-32%, 25-36%, 0.8-2%, 0.2-1.4%.
3, according to the described a kind of pentadiene graft copolymers synthetic method of claim 1, it is characterized in that the pentadiene copolymer temperature of fusion is 110 ℃-160 ℃, the time is 10-40 minute; Polymeric reaction temperature is 120 ℃-155 ℃, and the time is 3-20 minute; Melting temperature is 40 ℃-100 ℃, time 5-15 minute.
4, according to claim 1 or 2 described a kind of pentadiene graft copolymers synthetic methods, it is characterized in that strengthening agent is titanium dioxide and light calcium carbonate mixture; Coupling agent is vinyl three (β-oxyethyl group) silane; Oxidation inhibitor is 1010 oxidation inhibitor and the attached aid anti-oxidants of LDTP.
5, according to the described a kind of pentadiene graft copolymers synthetic method of claim 4, it is characterized in that titanium dioxide is 1: 3 with light calcium carbonate content ratio in the strengthening agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94114277 CN1125735A (en) | 1994-12-30 | 1994-12-30 | Synethsis method of pentadiene graft copolymer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94114277 CN1125735A (en) | 1994-12-30 | 1994-12-30 | Synethsis method of pentadiene graft copolymer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1125735A true CN1125735A (en) | 1996-07-03 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94114277 Pending CN1125735A (en) | 1994-12-30 | 1994-12-30 | Synethsis method of pentadiene graft copolymer |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415789C (en) * | 2006-06-21 | 2008-09-03 | 山西省应用化学研究所 | Dicyclopentadiene-rosin polymer and its prepn and application |
-
1994
- 1994-12-30 CN CN 94114277 patent/CN1125735A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100415789C (en) * | 2006-06-21 | 2008-09-03 | 山西省应用化学研究所 | Dicyclopentadiene-rosin polymer and its prepn and application |
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