CN112625248A - Organic silicon nylon elastomer and preparation method thereof - Google Patents
Organic silicon nylon elastomer and preparation method thereof Download PDFInfo
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- CN112625248A CN112625248A CN202011062592.1A CN202011062592A CN112625248A CN 112625248 A CN112625248 A CN 112625248A CN 202011062592 A CN202011062592 A CN 202011062592A CN 112625248 A CN112625248 A CN 112625248A
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- nylon
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 44
- 239000000806 elastomer Substances 0.000 title claims abstract description 43
- 239000004677 Nylon Substances 0.000 title claims abstract description 35
- 229920001778 nylon Polymers 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 12
- 239000010703 silicon Substances 0.000 title claims abstract description 12
- 229920002302 Nylon 6,6 Polymers 0.000 claims abstract description 26
- 150000003839 salts Chemical class 0.000 claims abstract description 22
- 229920001558 organosilicon polymer Polymers 0.000 claims abstract description 16
- 239000002535 acidifier Substances 0.000 claims abstract description 14
- 239000003054 catalyst Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 6
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 6
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 230000002087 whitening effect Effects 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- SCVFZCLFOSHCOH-UHFFFAOYSA-M potassium acetate Chemical compound [K+].CC([O-])=O SCVFZCLFOSHCOH-UHFFFAOYSA-M 0.000 claims description 18
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000006116 polymerization reaction Methods 0.000 claims description 9
- 235000011056 potassium acetate Nutrition 0.000 claims description 9
- 235000011037 adipic acid Nutrition 0.000 claims description 8
- 239000001361 adipic acid Substances 0.000 claims description 8
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 8
- -1 polydimethylsiloxane Polymers 0.000 claims description 8
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 8
- 238000007599 discharging Methods 0.000 claims description 7
- 229920000642 polymer Polymers 0.000 claims description 7
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- HVLLSGMXQDNUAL-UHFFFAOYSA-N triphenyl phosphite Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)OC1=CC=CC=C1 HVLLSGMXQDNUAL-UHFFFAOYSA-N 0.000 claims description 6
- OKOBUGCCXMIKDM-UHFFFAOYSA-N Irganox 1098 Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)NCCCCCCNC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 OKOBUGCCXMIKDM-UHFFFAOYSA-N 0.000 claims description 5
- RTBFRGCFXZNCOE-UHFFFAOYSA-N 1-methylsulfonylpiperidin-4-one Chemical compound CS(=O)(=O)N1CCC(=O)CC1 RTBFRGCFXZNCOE-UHFFFAOYSA-N 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 3
- 150000007513 acids Chemical class 0.000 claims description 3
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- 238000001953 recrystallisation Methods 0.000 claims description 3
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 3
- 239000002861 polymer material Substances 0.000 abstract description 2
- 238000005303 weighing Methods 0.000 abstract description 2
- 230000020477 pH reduction Effects 0.000 description 5
- 239000000203 mixture Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 150000002170 ethers Chemical class 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012661 block copolymerization Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/42—Block-or graft-polymers containing polysiloxane sequences
- C08G77/452—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences
- C08G77/455—Block-or graft-polymers containing polysiloxane sequences containing nitrogen-containing sequences containing polyamide, polyesteramide or polyimide sequences
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G69/00—Macromolecular compounds obtained by reactions forming a carboxylic amide link in the main chain of the macromolecule
- C08G69/48—Polymers modified by chemical after-treatment
Abstract
The invention provides an organic silicon nylon elastomer and a preparation method thereof, relating to the technical field of high polymer material preparation. The organic silicon nylon elastomer is prepared by weighing the following raw materials in parts by weight: 6000g-9000g of nylon 66 salt, 200g-1000g of acidifying agent, 800g-3000g of low-viscosity organic silicon polymer, 6 g-12 g of catalyst, 3 g-6 g of whitening agent and 3 g-6 g of antioxidant. The invention has the advantages of good impact resistance, obviously reduced hardness, gradually increased elongation at break up to 700% at most, belongs to a high-elasticity material, greatly improved elongation at break and rebound resilience compared with the traditional elastomer, and better flexibility of the novel nylon elastomer.
Description
Technical Field
The invention relates to the technical field of preparation of high polymer materials, in particular to an organic silicon nylon elastomer and a preparation method thereof.
Background
Nylon is a hard material with high strength, high wear resistance and high hardness, is mainly applied to the field of engineering plastics with high requirements on strength, and is limited in application in the field of elastomers, particularly in the field of high-flexibility elastomer materials due to low elasticity. In order to further expand the application range of the elastomer, the nylon elastomer is a product which is relatively hot to research in the industry at present and is also relatively high in applicability, block copolymerization polymerization is generally carried out by taking nylon as a hard segment and ethers as a soft segment, and the product has the characteristics of rubber and thermoplastic plastics and is favored in the fields of various elastomers. However, with the intensive research on nylon elastomers, products using ethers as soft segments have the problems of low elongation at break, low elasticity and the like, and in order to solve the problems of ether nylon elastomers, the development of an organosilicon nylon elastomer is urgently needed.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides an organosilicon nylon elastomer and a preparation method thereof, which solve the problems of low elongation at break, low elasticity and the like of nylon.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme: an organic silicon nylon elastomer is prepared by weighing the following raw materials in parts by weight: 6000g-9000g of nylon 66 salt, 200g-1000g of acidifying agent, 800g-3000g of low-viscosity organic silicon polymer, 6 g-12 g of catalyst, 3 g-6 g of whitening agent and 3 g-6 g of antioxidant.
Preferably, the nylon 66 salt is a crystal salt prepared by a recrystallization method, the acidifying agent is one of dibasic acids such as adipic acid and glutaric acid, the acidifying process is to completely dissolve the nylon 66 salt and then add the acidifying agent to make the mixture uniform, the low-viscosity organosilicon polymer is hydroxy-terminated polydimethylsiloxane, the viscosity is 100-500mpa.s, and the fluidity of the low-viscosity organosilicon polymer is ensured, the catalyst is one or a combination of two of potassium acetate, dibutyltin dilaurate and tetrabutyl titanate, and the nylon brightener is one of phosphorous acid, sodium hypophosphite and triphenyl phosphite.
Preferably, the preparation method of the silicone nylon elastomer comprises the following preparation methods:
s1, dissolving nylon 66 salt with softened water, adjusting the concentration of the solution to 65%, completely dissolving, adding 200g of an acidifier, and adjusting the acidity;
s2, adding a low-viscosity organic silicon polymer with the viscosity of 100-500mpa.s, a catalyst, a whitening agent and a 1098 type antioxidant, putting into a polymerization kettle, keeping the temperature and the pressure to 215 ℃ and 2.0Mpa, then gradually reducing the pressure to normal pressure, expelling gas at the normal pressure for 1 hour, and maintaining the vacuum degree to be-0.003 Mpa for 1 hour;
s3, discharging is carried out subsequently to obtain the nylon 66 elastomer, so that the hardness of the material is effectively reduced, the elongation at break is improved, and the processability is excellent.
Preferably, the nylon segment is taken as an X segment, the organic silicon polymer segment is taken as a Y segment, and water generated by the reaction is removed under certain temperature and pressure to form a segmented polymer, so that the elastomer polymer is obtained.
Preferably, the preparation method of the silicone nylon elastomer is a block reaction principle, and the reaction principle is as follows:
(III) advantageous effects
The invention provides an organosilicon nylon elastomer and a preparation method thereof. The method has the following beneficial effects:
1. the organosilicon polymer is introduced as a soft segment, so that the shock resistance is good, the hardness is obviously reduced, the elongation at break is gradually improved to be 600 percent at most, the elastomer belongs to a high-elasticity material, and the elongation at break and the rebound resilience are greatly improved compared with the traditional elastomer.
2. The invention prepares the novel nylon elastomer by taking organic silicon as a soft segment, and the novel nylon elastomer has better flexibility because the organic silicon long-chain polymer is a colloid flowing material with the advantages of controllable molecular weight, soft chain segment, simple acquisition, high yield and the like.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making an invasive operation based on the embodiments of the present invention, belong to the protection scope of the present invention.
The first embodiment is as follows:
the embodiment of the invention provides an organic silicon nylon elastomer, which is prepared from the following raw materials in parts by weight: 9000g of nylon 66 salt, 200g of an acidifying agent, 800g of a low-viscosity organic silicon polymer, 6g of a catalyst, 3g of a whitening agent and 3g of an antioxidant.
The nylon 66 salt is a crystal salt prepared by a recrystallization method, the acidifying agent is one of dibasic acids such as adipic acid, glutaric acid and the like, the acidifying process is to completely dissolve the nylon 66 salt and then add the acidifying agent to ensure the nylon 66 salt to be uniform, the low-viscosity organic silicon polymer is hydroxy-terminated polydimethylsiloxane, the viscosity is 100-one and 500mpa.s, the fluidity of the nylon 66 salt is ensured, the catalyst is one or the combination of two of potassium acetate, dibutyltin dilaurate and tetrabutyl titanate, and the nylon brightener is one of phosphorous acid, sodium hypophosphite and triphenyl phosphite.
A preparation method of a silicone nylon elastomer comprises the following preparation methods:
s1, dissolving 9000g of nylon 66 salt in softened water, adjusting the concentration of the solution to 65%, completely dissolving, adding 200g of adipic acid for acidification, and adjusting the acidity;
s2, adding 800g of hydroxyl-terminated polydimethylsiloxane with the viscosity of 500mpa.s, 3g of potassium acetate, 3g of tetrabutyl titanate, 3g of phosphorous acid and 3g of 1098 type antioxidant, putting into a polymerization kettle, keeping the temperature and the pressure to 215 ℃ and 2.0Mpa, then gradually reducing the pressure to normal pressure, driving gas at normal pressure for 1 hour, and maintaining the vacuum degree to be-0.003 Mpa for 1 hour;
s3, discharging is carried out subsequently to obtain the nylon 66 elastomer, so that the hardness of the material is effectively reduced, the elongation at break is improved, and the processability is excellent.
The nylon chain segment is taken as an X segment, the organic silicon polymer chain segment is taken as a Y segment, and water generated by the reaction is removed under certain temperature and pressure to form a segmented polymer, so that the elastomer polymer is obtained.
The preparation method of the organic silicon nylon elastomer is a segmented reaction principle, and the reaction principle is as follows:
example two:
dissolving 8000g of nylon 66 salt with softened water, adjusting the concentration of the solution to 65%, completely dissolving, adding 400g of adipic acid for acidification, adjusting the acidity, adding 1600g of hydroxyl-terminated polydimethylsiloxane with the viscosity of 500mpa.s, 4g of potassium acetate, 4g of tetrabutyl titanate, 4g of phosphorous acid and 4g of antioxidant 1098, putting into a polymerization kettle, keeping the temperature and the pressure at 215 ℃ and 2.0Mpa, gradually reducing the pressure to normal pressure, expelling gas at the normal pressure for 1 hour, maintaining the vacuum degree at-0.003 Mpa, and discharging to obtain the nylon 66 elastomer.
Example three:
dissolving 7500g of nylon 66 salt with softened water, adjusting the concentration of the solution to 65%, completely dissolving, adding 600g of adipic acid for acidification, adjusting the acidity, adding 1900g of hydroxyl-terminated polydimethylsiloxane with the viscosity of 500mpa.s, 5g of potassium acetate, 5g of tetrabutyl titanate, 5g of phosphorous acid and 5g of antioxidant 1098, putting into a polymerization kettle, keeping the temperature and the pressure at 215 ℃ and 2.0Mpa, then gradually reducing the pressure to the normal pressure, expelling gas at the normal pressure for 1 hour, maintaining the vacuum degree at-0.003 Mpa, and discharging to obtain the nylon 66 elastomer.
Example four:
7000g of nylon 66 salt is dissolved by softened water, the concentration of the solution is adjusted to 65%, the solution is completely dissolved, 800g of adipic acid is added for acidification, after the acidity is adjusted, 2200g of hydroxyl-terminated polydimethylsiloxane with the viscosity of 500mpa.s, 5g of potassium acetate, 5g of tetrabutyl titanate, 5g of phosphorous acid and 5g of antioxidant 1098 are added, the mixture is put into a polymerization kettle, the temperature and the pressure are kept at 215 ℃ and 2.0Mpa, then the pressure is gradually reduced to normal pressure, gas is removed for 1 hour at the normal pressure, the vacuum degree is kept at-0.003 Mpa, and the nylon 66 elastomer is obtained after 1 hour of discharging.
Example five:
6000g of nylon 66 salt is dissolved by softened water, the concentration of the solution is adjusted to 65 percent, after the solution is completely dissolved, 1000g of adipic acid is added for acidification, after the acidity is adjusted, 3000g of hydroxyl-terminated polydimethylsiloxane with the viscosity of 500mpa.s, 6g of potassium acetate, 6g of tetrabutyl titanate, 6g of phosphorous acid and 6g of antioxidant 1098 are added, the mixture is put into a polymerization kettle, the temperature and the pressure are kept at 215 ℃ and 2.0Mpa, then the pressure is gradually reduced to the normal pressure, the gas is removed for 1 hour at the normal pressure, the vacuum degree is kept at-0.003 Mpa, and the nylon 66 elastomer is obtained after the discharging.
The key performance indexes of the products produced by polymerization in each example are compared as shown in the table
| Serial number | Impact performance | Hardness of | Elongation at break |
| Example one | 25JNB | 111A | 150％ |
| Example two | 25JNB | 90A | 240％ |
| EXAMPLE III | 25JNB | 72A | 400％ |
| Example four | 25JNB | 58A | 550％ |
| Example four | 25JNB | 45A | 600％ |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The organic silicon nylon elastomer is characterized in that the raw materials are weighed according to the following formula in parts by weight: 6000g-9000g of nylon 66 salt, 200g-1000g of acidifying agent, 800g-3000g of low-viscosity organic silicon polymer, 6 g-12 g of catalyst, 3 g-6 g of whitening agent and 3 g-6 g of antioxidant.
2. The silicone nylon elastomer of claim 1, wherein: the nylon 66 salt is a crystal salt prepared by a recrystallization method, the acidifier is one of dibasic acids such as adipic acid and glutaric acid, the acidifier is added after the nylon 66 salt is completely dissolved in the acidifier to ensure the uniformity of the acidifier, the low-viscosity organic silicon polymer is hydroxy-terminated polydimethylsiloxane, the viscosity of the low-viscosity organic silicon polymer is 100-inch and 500-inch pa.s, the fluidity of the low-viscosity organic silicon polymer is ensured, the catalyst is one or the combination of two of potassium acetate, dibutyltin dilaurate and tetrabutyl titanate, and the nylon brightener is one of phosphorous acid, sodium hypophosphite and triphenyl phosphite.
3. A preparation method of an organosilicon nylon elastomer is characterized by comprising the following preparation methods:
s1, dissolving nylon 66 salt with softened water, adjusting the concentration of the solution to 65%, completely dissolving, adding 200g of an acidifier, and adjusting the acidity;
s2, adding a low-viscosity organic silicon polymer with the viscosity of 100-500mpa.s, potassium acetate, tetrabutyl titanate, a whitening agent and an antioxidant 1098 into a polymerization kettle, keeping the temperature and the pressure to 215 ℃ and 2.0MPa, then gradually reducing the pressure to normal pressure, expelling gas at the normal pressure for 1 hour, and maintaining the vacuum degree to be-0.003 Mpa for 1 hour;
s3, discharging is carried out subsequently to obtain the nylon 66 elastomer, so that the hardness of the material is effectively reduced, the elongation at break is improved, and the processability is excellent.
4. The method for preparing the silicone nylon elastomer according to claim 3, characterized in that: the nylon chain segment is taken as an X segment, the organic silicon polymer chain segment is taken as a Y segment, and water generated by the reaction is removed under certain temperature and pressure to form a segmented polymer, so that the elastomer polymer is obtained.
5. The method for preparing the silicone nylon elastomer according to claim 3, characterized in that: the preparation method of the organic silicon nylon elastomer is a segmented reaction principle, and the reaction principle is as follows:
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| CN202011062592.1A CN112625248A (en) | 2020-09-30 | 2020-09-30 | Organic silicon nylon elastomer and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113402713A (en) * | 2021-06-22 | 2021-09-17 | 湖北三宁碳磷基新材料产业技术研究院有限公司 | Preparation method of polyamide elastomer |
| CN113444243A (en) * | 2021-06-18 | 2021-09-28 | 山东东辰瑞森新材料科技有限公司 | Polyether-organic silicon composite nylon elastomer and preparation method thereof |
| CN113968966A (en) * | 2021-11-30 | 2022-01-25 | 万华化学集团股份有限公司 | Preparation method of nylon elastomer |
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| CN113968966A (en) * | 2021-11-30 | 2022-01-25 | 万华化学集团股份有限公司 | Preparation method of nylon elastomer |
| CN113968966B (en) * | 2021-11-30 | 2024-02-27 | 万华化学集团股份有限公司 | Preparation method of nylon elastomer |
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