CN105694093B - A kind of preparation method and application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system - Google Patents
A kind of preparation method and application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system Download PDFInfo
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- CN105694093B CN105694093B CN201610048447.5A CN201610048447A CN105694093B CN 105694093 B CN105694093 B CN 105694093B CN 201610048447 A CN201610048447 A CN 201610048447A CN 105694093 B CN105694093 B CN 105694093B
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 52
- 238000007142 ring opening reaction Methods 0.000 title claims abstract description 40
- 238000000605 extraction Methods 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 44
- 239000000654 additive Substances 0.000 claims abstract description 36
- 230000000996 additive effect Effects 0.000 claims abstract description 36
- 239000012141 concentrate Substances 0.000 claims abstract description 24
- 229910000406 trisodium phosphate Inorganic materials 0.000 claims abstract description 18
- 239000000243 solution Substances 0.000 claims abstract description 16
- 239000007853 buffer solution Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 12
- ALSPKRWQCLSJLV-UHFFFAOYSA-N azanium;acetic acid;acetate Chemical compound [NH4+].CC(O)=O.CC([O-])=O ALSPKRWQCLSJLV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005453 pelletization Methods 0.000 claims abstract description 6
- 238000006243 chemical reaction Methods 0.000 claims abstract description 4
- 239000000872 buffer Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 6
- 239000005695 Ammonium acetate Substances 0.000 claims description 5
- 229940043376 ammonium acetate Drugs 0.000 claims description 5
- 239000013078 crystal Substances 0.000 claims description 5
- USFZMSVCRYTOJT-UHFFFAOYSA-N Ammonium acetate Chemical compound N.CC(O)=O USFZMSVCRYTOJT-UHFFFAOYSA-N 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 4
- 235000019257 ammonium acetate Nutrition 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- 230000003068 static effect Effects 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 125000004122 cyclic group Chemical group 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 16
- 230000000694 effects Effects 0.000 abstract description 8
- 239000000047 product Substances 0.000 abstract description 8
- 230000002411 adverse Effects 0.000 abstract description 7
- 239000006227 byproduct Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 6
- 150000001875 compounds Chemical class 0.000 description 5
- 239000000178 monomer Substances 0.000 description 4
- 230000009467 reduction Effects 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007701 flash-distillation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 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 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
-
- 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
- C08G69/02—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids
- C08G69/08—Polyamides derived from amino-carboxylic acids or from polyamines and polycarboxylic acids derived from amino-carboxylic acids
- C08G69/14—Lactams
-
- 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
- C08G69/46—Post-polymerisation treatment
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Polyamides (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention provides a kind of preparation method and application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, and the ring opening agent system includes additive A and additive B, and the additive A is Na3PO4Solution, the additive B are acetic acid ammonium acetate buffer, the Na3PO4Concentration of polymer solution is 6%~10%, and the acetic acid ammonium acetate buffer solution pH is 4~7；Caprolactam polymerization is extracted after concentrate, additive A, additive B mix and carries out ring-opening reaction, the solution after reaction is used as with the mixing of fresh caprolactam polymerize required raw material；It will be mixed with modifying agent and delustering agent after the raw material preheating, subsequently into progress prepolymerization ring-opening reaction in prepolymerization tower, then wet slice obtained after whole poly-, pelletizing, centrifuge dripping.The present invention can reduce the higher adverse effect caused by product quality and equipment of cyclic oligomer content in current caprolactam polymerization extraction concentrate direct reuse technique, improve product quality, reduce production cost.
Description
【Technical field】
The present invention relates to the preparation method and application that a kind of caprolactam polymerization extracts concentration pendular ring aggressiveness ring opening agent system.
【Background technology】
At the end of caprolactam polymerization reaction, about containing 10% or so monomer and oligomer in reactant system,
Middle caprolactam about 70%, cyclic oligomer about 25%, linear oligomer about 5%.By extraction, these monomers and oligomer point
It is dispersed in extraction water.
In these monomers and oligomer, general monomer and linear oligomer have a higher reactivity, and cyclic oligomer
Then reactivity is relatively low, especially cyclic dimer, with the progress of reaction, gradually accumulates, seriously affects the quality of slice；And
And cyclic dimer bulk melting point is up to 340 DEG C or more, is easy to block pipeline, causes damage of facilities.
Extraction water recovery process has catalysis polymerization technology, oligomer cracking polymerization technique, concentrate direct reuse again at present
Technology, cyclic dimer biodegradation technique etc..For catalysis polymerization technology using second BASF AG as representative, they will extract concentrate
It is mixed to form solution with fresh caprolactam, heating, pressurization carry out prepolymerization by catalyst of metal oxide in fixed bed
Processing polymerize using flash distillation, decompression, and extractable significantly reduces in obtained slice；Concentrate cracking polymerize skill again
It is higher that art need to pass through processes, cost of equipment and the cost of technology such as high temperature phosphorous acid depolymerization, pre- water removal, rectifying；And concentrate directly returns
With in technology, directly participate in polymerizeing with the mixing of fresh caprolactam if concentrate is unprocessed, due to cyclic oligomer levels
Accumulation product quality and equipment can be adversely affected, while raw material availability is not also high.
Therefore, cyclic oligomer open loop again can be made under preheating temperature by finding one, and be reduced in pre-polymerization process
The substance or compound system that cyclic oligomer generates, to improving, product quality, to reduce cost significant.
【Invention content】
One of the technical problem to be solved in the present invention is to provide a kind of caprolactam polymerization extraction concentration pendular ring aggressiveness and opens
It is higher right can to reduce cyclic oligomer content in current caprolactam polymerization extraction concentrate direct reuse technique for ring agent system
Adverse effect caused by product quality and equipment improves product quality, reduces production cost.
The present invention is realized in one of above-mentioned technical problem：
A kind of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, the ring opening agent system includes additive A
And additive B, the main component of the additive A is Na3PO4The main component of solution, the additive B is acetic acid-ammonium acetate
Buffer solution.
Further, the Na3PO4Concentration of polymer solution is 6%~10%.
Further, the acetic acid-ammonium acetate buffer solution pH is 4~7.
The second technical problem to be solved by the present invention is to provide a kind of caprolactam polymerization extraction concentration pendular ring aggressiveness and opens
The preparation method of ring agent system can reduce cyclic oligomer in current caprolactam polymerization extraction concentrate direct reuse technique
The higher adverse effect caused by product quality and equipment of content, improves product quality, reduces production cost.
The present invention is realized in the twos' of above-mentioned technical problem：
A kind of preparation method of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, the ring opening agent system
Preparation method is as follows：
Step 1: desalted water is added in additive A surge-tank, and 90 DEG C are heated to, weigh the desired amount of Na3PO4It is brilliant
Body, in blanking to surge-tank, mechanical agitation is uniform, then is delivered in daily slot with pump and keeps the temperature 90 DEG C for use；
Step 2: desalted water is added in additive B surge-tank, and 80 DEG C are heated to, add ammonium acetate crystal, stirred,
And it is slowly added to a certain amount of glacial acetic acid, buffer solution is reconciled to required pH, is delivered to after stirring evenly in daily slot and is kept the temperature 80
It is DEG C for use.
The third technical problem to be solved by the present invention is to provide a kind of caprolactam polymerization extraction concentration pendular ring aggressiveness and opens
The application of ring agent system can reduce cyclic oligomer content in current caprolactam polymerization extraction concentrate direct reuse technique
The higher adverse effect caused by product quality and equipment, improves product quality, reduces production cost.
The present invention is realized in the threes' of above-mentioned technical problem：
A kind of application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, the application of the ring opening agent system
It is as follows：
By the good ring opening agent system of above-mentioned configuration, according to caprolactam polymerization extraction concentrate, additive A, additive B matter
Measuring score is respectively：2%~4%, 2%~4.5%, 91.5%~96% amount is delivered to reactor and carries out ring-opening reaction, institute
The control of reactor center temperature is stated at 150 DEG C, the solution after reaction is directly required former as polymerizeing with the mixing of fresh caprolactam
Material；Raw material preheating needed for polymerization is mixed with the modifying agent and delustering agent of caprolactam polymerization in static mixer to after 140 DEG C
It closes, subsequently into prepolymerization ring-opening reaction is carried out in prepolymerization tower, then obtains wet cut after whole poly-, pelletizing, centrifuge dripping again
Piece；
Further, the prepolymerization Open loop temperature is stablized at 243 DEG C~250 DEG C, final polymerization temperature stablize 250 DEG C~
255 DEG C, pelletizing coolant-temperature gage maintains about 14 DEG C.
Further, the Na3PO4Concentration of polymer solution is 6%~10%.
Further, the acetic acid-ammonium acetate buffer solution pH is 4~7.
The invention has the advantages that：
Problem to be solved by this invention is that cyclic oligomer content is higher in the current concentrate direct reuse technique of reduction
The adverse effect caused by product quality and equipment.The open loop system prepared using the present invention can make the content of cyclic oligomer
52% or so are reduced, while extractable reduction by 19% or so in wet slice is obtained after making centrifuge dripping, can be generated larger
Economic benefit.
Since present invention employs buffer solution and Na3PO4Open loop system as main component adapts to recycling fluid wave
Dynamic variation promotes ring aggressiveness open loop, and is reduced the effect of the formation of polymerization process middle ring polymers, to improving raw material profit
There is positive effect with rate and product quality, and production cost can be substantially reduced.
【Description of the drawings】
The present invention is further illustrated in conjunction with the embodiments with reference to the accompanying drawings.
Fig. 1 is the technique for applying flow diagram of the method for the present invention.
【Specific implementation mode】
Refering to Figure 1, the embodiment of the present invention is described in detail.
As shown in Figure 1, a kind of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system according to the present invention,
It is characterized in that：The ring opening agent system includes additive A and additive B, and the main component of the additive A is Na3PO4Solution,
The main component of the additive B is acetic acid-ammonium acetate buffer.The Na3PO4Concentration of polymer solution is 6%~10%.Institute
It is 4~7 to state acetic acid-ammonium acetate buffer solution pH.
The invention further relates to a kind of preparation method of above-mentioned caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system,
The preparation method of the ring opening agent system is as follows：
Step 1: desalted water is added in additive A surge-tank, and 90 DEG C are heated to, weigh the desired amount of Na3PO4It is brilliant
Body, in blanking to surge-tank, mechanical agitation is uniform, then is delivered in daily slot with pump and keeps the temperature 90 DEG C for use；
Step 2: desalted water is added in additive B surge-tank, and 80 DEG C are heated to, add ammonium acetate crystal, stirred,
And it is slowly added to a certain amount of glacial acetic acid, buffer solution is reconciled to required pH, is delivered to after stirring evenly in daily slot and is kept the temperature 80
It is DEG C for use.
The present invention further relates to a kind of application of above-mentioned caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, described
The application of ring opening agent system is as follows：
By the good ring opening agent system of above-mentioned configuration, according to caprolactam polymerization extraction concentrate/additive A/additive B=
100/2.5/2.5 mass ratio is delivered to reactor and carries out ring-opening reaction, and the reactor center temperature control is at 150 DEG C, instead
Solution after answering, which is directly used as with the mixing of fresh caprolactam, polymerize required raw material；Will raw material preheating needed for polymerization to after 140 DEG C
It is mixed in static mixer with the modifying agent of caprolactam polymerization and delustering agent, subsequently into carrying out prepolymerization in prepolymerization tower
Then ring-opening reaction obtains wet slice after whole poly-, pelletizing, centrifuge dripping again.
The prepolymerization Open loop temperature is stablized at 243 DEG C~250 DEG C, and final polymerization temperature is stablized at 250 DEG C~255 DEG C, cuts
Grain coolant-temperature gage maintains about 14 DEG C.
The ring opening agent system is applied to the extraction concentrate for the recovered liquid that caprolactam returns after polymerisation, by acyl in oneself
After amine polymerization extraction concentrate carries out open loop, rejoins fresh caprolactam and carrying out a new wheel polymerisation.
Below by embodiment, the present invention is further elaborated.
Embodiment 1
A certain amount of desalted water is added in additive A surge-tank, and is heated to 90 DEG C, weighs desalination water quality 7%
Na3PO4Crystal, in blanking to surge-tank, mechanical agitation 1h, then be delivered in daily slot with pump and keep the temperature 90 DEG C for use.
A certain amount of desalted water is added in additive B surge-tank, and is heated to 80 DEG C, it is brilliant to add a certain amount of ammonium acetate
Body opens stirring, and is slowly added to glacial acetic acid, reconciles buffer solution to pH=7, is delivered in daily slot and keeps the temperature after stirring evenly
80 DEG C for use.
By the good ring opening agent system of above-mentioned configuration, according to caprolactam polymerization extraction concentrate/additive A/additive B=
100/2.5/2.5 mass ratio is delivered to tubular reactor and carries out ring-opening reaction, and tubular reactor central temperature is controlled 150
DEG C, the solution after ring-opening reaction is directly with the mixing of fresh caprolactam as required raw material is polymerize, by the raw material preheating to 140 DEG C
It is mixed in static mixer with the modifying agent of caprolactam polymerization and delustering agent afterwards, it is anti-subsequently into being carried out in prepolymerization tower
It answers, then obtains wet slice after whole poly-, pelletizing, centrifuge dripping again.Prepolymerization Open loop temperature is stablized at 243 DEG C~250 DEG C, pressure
Power is stablized in 1500mbar or so；Final polymerization VK tube temperature degree is stablized at 250 DEG C~255 DEG C, and pressure stability is cut in 1296mbara
Grain water enters coolant-temperature gage and maintains about 14 DEG C.Detailed process is shown in Fig. 1
After testing, by the open loop system treated concentrate, caprolactam about 71.05%, cyclic oligomer are about
13.25%, linear oligomer about 15.70%.
Embodiment 2
It is operated according to the preparation method and polymerization technique of embodiment 1, except that Na3PO4Mass concentration be
8.5%, the pH of acetic acid-ammonium acetate buffer solution is 6.5.
After testing, by the compound open loop system treated concentrate, caprolactam about 71.10%, cyclic oligomer
Object about 12.75%, linear oligomer about 16.15%.
Embodiment 3
It is operated according to the preparation method and polymerization technique of embodiment 1, except that Na3PO4Mass concentration be
8.5%, the pH of acetic acid-ammonium acetate buffer solution is 5.5.
After testing, by the compound open loop system treated concentrate, caprolactam about 71.15%, cyclic oligomer
Object about 12.25%, linear oligomer about 16.60%.
Embodiment 4
It is operated according to the preparation method and polymerization technique of embodiment 1, except that Na3PO4Mass concentration be
7.5%, the pH of acetic acid-ammonium acetate buffer solution is 5.5.
After testing, by the compound open loop system treated concentrate, caprolactam about 71.17%, cyclic oligomer
Object about 12.75%, linear oligomer about 16.83%.
Embodiment 5
It is operated according to the preparation method and polymerization technique of embodiment 1, except that caprolactam polymerization extraction is dense
Contracting liquid, additive A, additive B mass fraction are respectively：3%, 2%, 95%.
After testing, by the compound system treated concentrate, caprolactam about 71.23%, cyclic oligomer are about
13.15%, linear oligomer about 15.62%.
Problem to be solved by this invention is that cyclic oligomer content is higher in the current concentrate direct reuse technique of reduction
The adverse effect caused by product quality and equipment.The open loop system prepared using the present invention can make the content of cyclic oligomer
52% or so are reduced, while extractable reduction by 19% or so in wet slice is obtained after making centrifuge dripping, can be generated larger
Economic benefit.
Since present invention employs buffer solution and Na3PO4Open loop system as main component adapts to recycling fluid wave
Dynamic variation promotes ring aggressiveness open loop, and is reduced the effect of the formation of polymerization process middle ring polymers, to improving raw material profit
There is positive effect with rate and product quality, and production cost can be substantially reduced.
Although specific embodiments of the present invention have been described above, those familiar with the art should manage
Solution, we are merely exemplary described specific embodiment, rather than for the restriction to the scope of the present invention, it is familiar with this
The technical staff in field modification and variation equivalent made by the spirit according to the present invention, should all cover the present invention's
In scope of the claimed protection.
Claims (4)
1. a kind of preparation method of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, it is characterised in that：It is described to open
The preparation method of ring agent system is as follows：
Step 1: desalted water is added in additive A surge-tank, and 90 DEG C are heated to, weigh the desired amount of Na3PO4Crystal, under
In material to surge-tank, mechanical agitation is uniform, then is delivered in daily slot with pump and keeps the temperature 90 DEG C for use；
Step 2: desalted water is added in additive B surge-tank, and 80 DEG C are heated to, add ammonium acetate crystal, stirring, and delay
Slowly a certain amount of glacial acetic acid is added, reconciles buffer solution to required pH, 80 DEG C of heat preservation in daily slot is delivered to after stirring evenly and is waited for
With；
The ring opening agent system includes additive A and additive B, and the main component of the additive A is Na3PO4Solution, it is described
The main component of additive B is acetic acid-ammonium acetate buffer；The Na3PO4Concentration of polymer solution is 6%~10%, the vinegar
Acid-ammonium acetate buffer solution pH is 4~7.
2. a kind of application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system, it is characterised in that：The ring opening agent
System is prepared by a kind of preparation method of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system described in claim 1
, the application of the ring opening agent system is as follows：
By the good ring opening agent system of above-mentioned configuration, it is delivered to after being mixed with caprolactam extraction concentrate according to certain mass ratio anti-
Answer device to carry out ring-opening reaction, reactor center temperature control at 150 DEG C, solution after reaction directly with fresh caprolactam
Mixing is as raw material needed for polymerization；By raw material preheating needed for polymerization to caprolactam polymerization after 140 DEG C modifying agent and delustring
Agent mixes in static mixer, subsequently into prepolymerization ring-opening reaction is carried out in prepolymerization tower, then again through poly-, pelletizing eventually,
Wet slice is obtained after centrifuge dripping.
3. a kind of application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system according to claim 2,
It is characterized in that：Caprolactam polymerization extraction concentrate, additive A, additive B mass fraction are respectively：2%~4%, 2%~
4.5%, 91.5%~96%.
4. a kind of application of caprolactam polymerization extraction concentration pendular ring aggressiveness ring opening agent system according to claim 2,
It is characterized in that：The prepolymerization Open loop temperature is stablized at 243 DEG C~250 DEG C, and final polymerization temperature is stablized at 250 DEG C~255 DEG C, cuts
Grain coolant-temperature gage is maintained 14 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1345889A (en) * | 2000-09-29 | 2002-04-24 | 巴陵石化岳阳石油化工总厂 | Method for producing polyamide 6 section |
| CN103159951A (en) * | 2011-12-13 | 2013-06-19 | 上海杰事杰新材料(集团)股份有限公司 | Method and apparatus for preparing high temperature nylon |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1345889A (en) * | 2000-09-29 | 2002-04-24 | 巴陵石化岳阳石油化工总厂 | Method for producing polyamide 6 section |
| CN103159951A (en) * | 2011-12-13 | 2013-06-19 | 上海杰事杰新材料(集团)股份有限公司 | Method and apparatus for preparing high temperature nylon |
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