CN106188542A - A kind of manufacture method of heat resistance corrosion-resistant polyphenylene sulfide ketone - Google Patents
A kind of manufacture method of heat resistance corrosion-resistant polyphenylene sulfide ketone Download PDFInfo
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- CN106188542A CN106188542A CN201610778158.0A CN201610778158A CN106188542A CN 106188542 A CN106188542 A CN 106188542A CN 201610778158 A CN201610778158 A CN 201610778158A CN 106188542 A CN106188542 A CN 106188542A
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- Prior art keywords
- polyphenylene sulfide
- heat resistance
- manufacture method
- corrosion
- solvent
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- 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
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/0204—Polyarylenethioethers
- C08G75/025—Preparatory processes
- C08G75/0254—Preparatory processes using metal sulfides
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- 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
- C08G75/00—Macromolecular compounds obtained by reactions forming a linkage containing sulfur with or without nitrogen, oxygen, or carbon in the main chain of the macromolecule
- C08G75/02—Polythioethers
- C08G75/0204—Polyarylenethioethers
- C08G75/0236—Polyarylenethioethers containing atoms other than carbon or sulfur in a linkage between arylene groups
- C08G75/024—Polyarylenethioethers containing atoms other than carbon or sulfur in a linkage between arylene groups containing carbonyl groups
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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)
- Polymers With Sulfur, Phosphorus Or Metals In The Main Chain (AREA)
Abstract
The invention discloses the manufacture method of a kind of heat resistance corrosion-resistant polyphenylene sulfide ketone, including raw material: sodium sulfide, 4.4 1 dichlorobenzophenone, paracide, solvent: n methyl is solvent than pyrrolidone, auxiliary agent: sodium hydroxide, catalyst；Being primarily characterized in that: described raw material obtains polymer with solvent, auxiliary agent, polymerization catalyst after reacting, can collect precipitate after polymer cooling, precipitate is size-reduced, wash, obtain product after drying；The good stability of the method, favorable reproducibility, solve resulting polymers quality unstable, the problem that molecular weight is the biggest, improve the properties of the degree of polymerization and polymer.
Description
Technical field
The present invention relates to macromolecule resin synthesis technical field, especially relate to a kind of corrosion-resistant polyphenylene sulfide of heat resistance
The manufacture method of ketone.
Background technology
Engineering plastics are widely used in electric, automobile, building, office equipment, machinery, Aero-Space etc. in recent years
Industry, to mould Dai Gang, to become international popular trend moulding Dai Muyi.Engineering plastics have become in world today's plastics industry and have increased
Fastest field, its development not only plays supporting role to country's pillar industry and modern high technology industry, the most also
Promoting Transform of Traditional Industrial Equipment and the adjustment of product structure, polyphenylene sulfide (PPS) then belongs to the one of engineering plastics.
Polyphenylene sulfide (PPS) is the special engineering plastics of a kind of excellent combination property.It is strong that polyphenylene sulfide (PPS) has machinery
Spend high, high temperature resistant, high fire-retardance, hard and crisp, degree of crystallinity is high, electrical property is excellent, chemical resistance is strong, and chemical resistance is only second to
Politef, mobility is only second to nylon, and light transmittance is only second to the advantages such as lucite, coloring resistance to water；By adding glass
The advantages such as glass fiber or other reinforcing material are modified, and impact strength can be made to greatly improve, and the tired property of vibration resistance is good.State-owned enterprise of state
Industry is actively researched and developed, and has preliminarily formed certain production capacity, changes the situation being in the past completely dependent on import.
But, domestic polyphenylene sulfide (PPS) technology there is also that product variety functional product few, high is few, production capacity is anxious waits to expand
Etc. problem, these are the Important Problems obstructing next step development of polyphenylene sulfide (PPS).Develop high temperature resistant, corrosion-resistant, high intensity,
The engineering plastics of high-modulus are always the big event in field of polymer technology, and polyphenylene sulfide ketone is as a kind of new in this resinoid
The material of type, is just equipped with a feature that, which overcomes polyphenylene sulfide molecular weight relatively low, colour-difference, and mechanical performance is imperfect
Problem.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of heat resistance corrosion-resistant polyphenylene sulfide ketone
Manufacture method, the molecular weight solving the existence of above-mentioned resin is relatively low, colour-difference, the imperfect problems and disadvantages of mechanical performance, this
Bright being dehydrated by employing, the method for high-pressure charging and LP synthesizing synthesizes colory new type resin.
The technical solution adopted in the present invention is: the manufacture method of a kind of heat resistance corrosion-resistant polyphenylene sulfide ketone, including
Raw material: sodium sulfide, 4.4 1 dichlorobenzophenone, paracide, solvent: n-methyl is than pyrrolidone, auxiliary agent: sodium hydroxide, catalysis
Agent；It is primarily characterized in that: described sodium sulfide is 1.03:0.7 with the mol ratio of paracide and 4.4 1 dichlorobenzophenone:
0.3；Described raw material obtains polymer with solvent, auxiliary agent, polymerization catalyst after reacting, can collect precipitate after polymer cooling,
Precipitate is size-reduced, wash, obtain product after drying；Described raw material with solvent, auxiliary agent, the polymeric reaction temperature of catalyst is
150～280 DEG C, pressure condition is 0～1 m Pa, and required time is 4h-9h.
Further illustrate, described raw material sodium sulfide and solvent n-methyl than pyrrolidone, auxiliary agent sodium hydroxide, catalyst de-
Coolant-temperature gage is 150～170 DEG C, and dewatering time is 2 hours, and is sequentially added into 4.4 1 dichlorobenzophenone, reacts after paracide
To prepolymer.
Further illustrating, during the reaction of described prepolymer a length of 2～4 hours, temperature required is 170 ° of C-230 ° of C, reaction
After obtain polymer solution.
Further illustrate, during the reaction of described polymer solution a length of 2～3 hours, temperature required be 230 ° of C-280 ° of C,
Pressure is 0～1Mpa.
Further illustrating, described precipitate through stopped reaction by polymer solution, and is cooled to 120 ° of below C and generates.
Further illustrating, described product is, washing size-reduced by centrifugation precipitate out, the product that obtains after drying
Thing.
Compared with prior art, the invention has the beneficial effects as follows: the manufacture of a kind of heat resistance corrosion-resistant polyphenylene sulfide ketone
Method, by the method for polymerization under normal pressure charging by several times and low pressure, the resin property of synthesis is stable, in normal pressure charging by several times, is
Polyreaction is reacted in a temperature range, and normal pressure charging by several times makes polymer reaction react in certain temperature range, has
The effect bumping that anti-thermal response causes when preventing polymerization, in periods of low pressure, promotes heavy polymer anti-of oligomer
Should, improve the properties of the degree of polymerization and polymer.
Accompanying drawing explanation
Fig. 1 is the flow chart of the present invention.
Detailed description of the invention
The present invention is further described below in conjunction with the accompanying drawings.
As it is shown in figure 1, include raw material: sodium sulfide, 4.4 1 dichlorobenzophenone, paracide, solvent: n-methyl ratio coughs up alkane
Ketone, auxiliary agent: sodium hydroxide, catalyst；It is primarily characterized in that: described sodium sulfide and paracide and 4.4 1 dichlorobenzophenone
Mol ratio be 1.03:0.7:0.3；Described raw material obtains polymer, polymer with solvent, auxiliary agent, polymerization catalyst after reacting
Can collect precipitate after cooling, precipitate is size-reduced, wash, obtain product after drying；Described raw material and solvent, auxiliary agent, catalysis
The polymeric reaction temperature of agent is 150～280 DEG C, and pressure condition is 0～1 m Pa, and required time is 4h-9h.
Specific implementation process is as follows:
One, in magnetic force reactor, add solvent: n-methyl than pyrrolidone, auxiliary agent: sodium hydroxide, catalyst, and raw material:
Sodium sulfide, heated and stirred, it is dehydrated 2 hours under the conditions of 150～170 DEG C after stirring, adds paracide and 4.4 1 by several times
Dichlorobenzophenone, then react 2～4 hours under the conditions of 170～230 DEG C, generate prepolymer.
Two, under prepolymer state, regulating pressure to 0～1MPa, temperature controls under the conditions of 230～280 degree Celsius,
React 2～3 hours and generate polymer solution.
Three, stopped reaction, cools the temperature to less than 120 degree Celsius, collects precipitate through centrifugation after cooling, then through powder
Broken, wash, be dried thus obtain product.
The present invention uses the method for polymerization under normal pressure charging by several times and low pressure compared to conventional art, organically conventional skill
Art is combined, and the resin property of synthesis is stable, improves temperature tolerance, corrosion resistance and modulus, and polymerization time is shorter, with
Time mechanical performance be greatly improved, cost is greatly reduced, and has wide marketing effect.
As known by the technical knowledge, the present invention can realizing without departing from the technical program by other, the most described herein,
Being only presently preferred embodiments of the present invention, not in order to limit the present invention, all within design concept of the present invention, that is made appoints
What amendment, equivalent, improvement etc., should be included within the scope of the present invention.
Claims (6)
1. a manufacture method for heat resistance corrosion-resistant polyphenylene sulfide ketone, including raw material: sodium sulfide, 4.4 1 dichlorobenzophenone,
Paracide, solvent: n-methyl is than pyrrolidone, auxiliary agent: sodium hydroxide, catalyst；It is characterized in that: described sodium sulfide with to two
The mol ratio of chlorobenzene and 4.4 1 dichlorobenzophenone is 1.03:0.7:0.3；Described raw material and solvent, auxiliary agent, being polymerized of catalyst
Reaction temperature is 150～280 DEG C, and pressure condition is 0～1 m Pa, and required time is 4h-9h, described raw material and solvent, auxiliary agent,
Obtaining polymer after polymerization catalyst reaction, can collect precipitate after polymer cooling, precipitate is size-reduced, washing, dried
Obtain product.
The manufacture method of a kind of heat resistance the most according to claim 1 corrosion-resistant polyphenylene sulfide ketone, it is characterised in that: institute
Stating raw material sodium sulfide with solvent n-methyl than pyrrolidone, auxiliary agent sodium hydroxide, the dehydration temperaturre of catalyst are 150～170 DEG C, de-
The water time is 2 hours, and is sequentially added into paracide, and after 4.4 1 dichlorobenzophenone, reaction obtains prepolymer.
The manufacture method of a kind of heat resistance the most according to claim 2 corrosion-resistant polyphenylene sulfide ketone, it is characterised in that: institute
Stating during the reaction of prepolymer a length of 2～4 hours, temperature required is 170 ° of C～230 ° of C, obtains polymer solution after reaction.
The manufacture method of a kind of heat resistance the most according to claim 3 corrosion-resistant polyphenylene sulfide ketone, it is characterised in that: institute
Stating during the reaction of polymer solution a length of 2～3 hours, temperature required is 230 ° of C～280 ° of C, pressure are 0～1Mpa.
The manufacture method of a kind of heat resistance the most according to claim 1 corrosion-resistant polyphenylene sulfide ketone, it is characterised in that: institute
State precipitate by polymer solution through stopped reaction, and cool to 120 ° of below C generations.
The manufacture method of a kind of heat resistance the most according to claim 1 corrosion-resistant polyphenylene sulfide ketone, it is characterised in that: institute
State product be, washing size-reduced by centrifugation precipitate out, the product that obtains after drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610778158.0A CN106188542A (en) | 2016-08-31 | 2016-08-31 | A kind of manufacture method of heat resistance corrosion-resistant polyphenylene sulfide ketone |
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| CN201610778158.0A CN106188542A (en) | 2016-08-31 | 2016-08-31 | A kind of manufacture method of heat resistance corrosion-resistant polyphenylene sulfide ketone |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0367470A2 (en) * | 1988-10-25 | 1990-05-09 | Kureha Kagaku Kogyo Kabushiki Kaisha | Stretched poly(arylene thioether) block copolymer films and production process thereof |
-
2016
- 2016-08-31 CN CN201610778158.0A patent/CN106188542A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0367470A2 (en) * | 1988-10-25 | 1990-05-09 | Kureha Kagaku Kogyo Kabushiki Kaisha | Stretched poly(arylene thioether) block copolymer films and production process thereof |
Non-Patent Citations (5)
| Title |
|---|
| 全国安全生产教育培训教材编审委员会组织: "《聚合工艺作业》", 30 April 2013, 中国矿业大学出版社 * |
| 李群等: "《高分子化学》", 31 August 1991, 成都科技大学出版社 * |
| 陈勇等: "《共聚物聚苯硫醚－聚苯硫醚酮的合成及表征》", 《化工新型材料》 * |
| 陈新等: "《PPSK/PPS共聚物的合成及其初步研究》", 《高分子材料科学与工程》 * |
| 马之庚等: "《工程塑料手册 材料卷》", 31 October 2004, 机械工业出版社 * |
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