CN1085918A - A kind of preparation method of modification of nylon - Google Patents
A kind of preparation method of modification of nylon Download PDFInfo
- Publication number
- CN1085918A CN1085918A CN 92107176 CN92107176A CN1085918A CN 1085918 A CN1085918 A CN 1085918A CN 92107176 CN92107176 CN 92107176 CN 92107176 A CN92107176 A CN 92107176A CN 1085918 A CN1085918 A CN 1085918A
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- nylon
- oligopolymer
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- weight ratio
- plastic
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Abstract
A kind of preparation method of modification of nylon, the present invention is a main raw material with depleted nylon 6 oligopolymer in the polyamide fibre production process, by with methyl-isobutyl acrylate, vinyl acetate between to for plastic is polymerization in polymeric kettle, form methyl-isobutyl acrylate-vinyl acetate between to for plastic-nylon 6 oligopolymer terpolymers and make modification of nylon, this modification of nylon is compared with similar resin, it is low to have water-absorbent, low temperature brittleness is improved, shrinking percentage is low, the advantage that internal stress is little, when being especially in use in big of castable plastic, product does not have steam bubble, mould can not heat, moulding at normal temperatures, also plastic under big humidity situation.
Description
The present invention relates to the preparation method of nylon.
Along with developing rapidly of polyamide fibre industry, waste-nylon 6 oligopolymer in the polyamide fibre production process are more and more, how it rationally utilized, begin to cause people's attention, as utilized nylon 6 oligopolymer to produce coating, but generally speaking, utilize also very undesirablely, value added is not high yet.
The object of the present invention is to provide a kind of method of utilizing depleted nylon 6 oligopolymer in the polyamide fibre production process to produce modification of nylon, this modification of nylon can be used for production machinery, electrical component, also can reel off raw silk from cocoons, and big of various plastics can also be used to cast.
The present invention is achieved in that
Place polymeric kettle to react with nylon 6 oligopolymer with by methyl-isobutyl acrylate, vinyl acetate between to for plastic, benzoyl peroxide, azide silane coupling agent blended prepolymer, form methyl-isobutyl acrylate-vinyl acetate between to for plastic-nylon 6 oligopolymer terpolymers.Make modification of nylon through cooling.
Describe the present invention in detail below in conjunction with embodiment.
Main raw material of the present invention derives from waste-nylon 6 oligopolymer that polyamide fibre industry and cord fabrics polymerization workshop section quench and get in the groove to be reclaimed in the later stage.It is a kind of mixture that contains hexanolactam and nylon 6, and its molecular structure is a following formula:
Nylon 6 oligopolymer inputs have been charged into nitrogen, temperature be controlled in 120 ° ± 10 ℃ the melt still, connected vacuum pump, progressively heated up, drying under reduced pressure, the drying under reduced pressure temperature-stable is controlled at 170 °-190 ℃, in the still negative regulation at 0.2MPa, ridity: require water content below 300PPm.After the nylon 6 oligopolymer dryings, charge into the nitrogen of 0.3MPa in still in the still, open blow-off valve at the bottom of the still, material is pressed into strainer, filtering net requires again filtered melt to be delivered to polymeric kettle more than 200 orders.Polymeric kettle is warming up to 170-190 ℃ before charging, and with nitrogen air in the still is drained only.The feeding quantity of polymeric kettle is no more than still volumetrical 2/3.Add the melt of nylon 6 oligopolymer at polymeric kettle after, the weight ratio 1-3 ‰ that presses nylon 6 oligopolymer added catalyst n aOH, 160-180 ℃ of decompression reaction 40-60 minute.After this, the prepolymer that adds methyl-isobutyl acrylate and vinyl acetate between to for plastic blend.
Prepolymer is prepared by following method:
Get methyl-isobutyl acrylate and the vinyl acetate between to for plastic that accounts for nylon 6 oligopolymer weight ratio 1-10% by nylon 6 oligopolymer weight ratio 1-5%, with its mixing, stirring, add that to account for the prepolymer weight ratio be 0.5～3% catalyzer benzoyl peroxide and to account for the prepolymer weight ratio be 0.5～5% solvent azide silane coupling agent, 45-55 ℃ of reaction 2-4 hour.
After adding prepolymer, 180-200 ℃ of reaction 40 minutes, add then that to account for the total amount weight ratio be 0.5～3% NaOH, reacted again 20 minutes at 190-210 ℃, add the promotor isocyanic ester that accounts for oligopolymer weight ratio 2-8 ‰, temperature is risen to 230-240 ℃ of reaction 1-2 hour.This moment, reaction was finished, when being reduced to 220 ℃, temperature in still, charges into the nitrogen of 0.2-0.4MPa, bleeder valve at the bottom of the polymeric kettle is opened, through the poly-stripping of taking the lead, cooling tank [1] through make cooling fluid with white oil flows to cooling tank [2] cooling, cooling tank [2] is made cooling fluid with Potassium ethanoate and water, and its ratio is 1.3: 1.Through the dicing machine pelletizing, centrifuge dehydration, vacuum-drying promptly obtain modification of nylon with cooled product.
The present invention compares with similar resin, and the advantage of have that water-absorbent is low, low temperature brittleness being improved, shrinking percentage is low, internal stress is little is when being especially in use in big of castable plastic, product does not have steam bubble, mould can not heat, and moulding at normal temperatures is also plastic under big humidity situation.
Claims (7)
1, a kind of preparation method of modification of nylon, feature of the present invention is to be raw material with 6 oligopolymer of the waste-nylon in the polyamide fibre production process, through drying under reduced pressure in the melt still and prepolymer polymerization in polymeric kettle of filtering the back and obtaining, make modification of nylon through cooling tank cooling, pelletizing, centrifuge dehydration, vacuum-drying by methyl-isobutyl acrylate, vinyl acetate between to for plastic, benzoyl peroxide, azide silane coupling agent uniform mixing.
2, by the described method of claim 1, it is characterized in that the drying under reduced pressure temperature-stable in the melt still is controlled at 170-190 ℃, negative regulation is at 0.2MPa in the still, water content is controlled at below the 300PPm, after the nylon 6 oligopolymer dryings, in still, charge into the nitrogen of 0.3MPa and material is pressed into strainer in the still.
3, by claim 1,2 described methods, the filtering net mesh that it is characterized in that strainer is more than 200 orders.
4, by the described method of claim 1, it is characterized in that prepolymer prepares as follows:
Get methyl-isobutyl acrylate and the vinyl acetate between to for plastic that accounts for nylon 6 oligopolymer weight ratio 1-10% by nylon 6 oligopolymer weight ratio 1-5%, with its mixing, stirring, add that to account for the prepolymer weight ratio be the benzoyl peroxide of 0.5-3% and account for the azide silane coupling agent that the prepolymer weight ratio is 0.5-5%, 45-55 ℃ of reaction 2-4 hour.
5, by the described method of claim 1, it is characterized in that after polymeric kettle adds the melt of nylon 6 oligopolymer, the weight ratio 1-3 ‰ that presses nylon 6 oligopolymer adds NaOH, 160-180 ℃ of decompression reaction 40-60 minute, add prepolymer again, 180-200 ℃ of reaction 40 minutes, add and account for the NaOH that the total amount weight ratio is 0.5-3%, 190-210 ℃ of reaction 20 minutes, add the isocyanic ester that accounts for oligopolymer weight ratio 2-8 ‰ again, temperature is risen to 230-240 ℃ of reaction 1-2 hour, temperature is reduced to 220 ℃ then and in still, charges into 0.2-0.4MPa nitrogen.
6, by claim 1,5 described methods, it is characterized in that polymeric kettle is warmed up to 170-190 ℃ before charging, and air in the still drained only that the feeding quantity of polymeric kettle is no more than still volumetrical 2/3 with nitrogen.
7, by the described method of claim 1, it is characterized in that cooling tank [1] with white oil as cooling fluid, as cooling fluid, its ratio is 1.3: 1 to cooling tank [2] with Potassium ethanoate and water.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107176 CN1085918A (en) | 1992-10-08 | 1992-10-08 | A kind of preparation method of modification of nylon |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92107176 CN1085918A (en) | 1992-10-08 | 1992-10-08 | A kind of preparation method of modification of nylon |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1085918A true CN1085918A (en) | 1994-04-27 |
Family
ID=4942729
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92107176 Pending CN1085918A (en) | 1992-10-08 | 1992-10-08 | A kind of preparation method of modification of nylon |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1085918A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049703C (en) * | 1996-11-04 | 2000-02-23 | 岳阳石油化工总厂研究院 | Method for producing nylon 6 by using caprolactam oligomer residue |
| CN104805536A (en) * | 2015-03-26 | 2015-07-29 | 巢湖市翔宇渔具有限公司 | Cooling liquid for drafting of fishing line |
| CN108424636A (en) * | 2018-01-29 | 2018-08-21 | 上海睿聚环保科技有限公司 | A kind of low-cost and high-performance regeneration daiamid composition modified materials |
| CN111438127A (en) * | 2020-03-05 | 2020-07-24 | 恒天纤维集团有限公司 | Low-temperature cleaning process for degradable nylon 4 |
-
1992
- 1992-10-08 CN CN 92107176 patent/CN1085918A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1049703C (en) * | 1996-11-04 | 2000-02-23 | 岳阳石油化工总厂研究院 | Method for producing nylon 6 by using caprolactam oligomer residue |
| CN104805536A (en) * | 2015-03-26 | 2015-07-29 | 巢湖市翔宇渔具有限公司 | Cooling liquid for drafting of fishing line |
| CN108424636A (en) * | 2018-01-29 | 2018-08-21 | 上海睿聚环保科技有限公司 | A kind of low-cost and high-performance regeneration daiamid composition modified materials |
| CN111438127A (en) * | 2020-03-05 | 2020-07-24 | 恒天纤维集团有限公司 | Low-temperature cleaning process for degradable nylon 4 |
| CN111438127B (en) * | 2020-03-05 | 2021-10-15 | 恒天纤维集团有限公司 | Low-temperature cleaning process for degradable nylon 4 |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |