CN107151278A - A kind of Corvic post-processing approach - Google Patents
A kind of Corvic post-processing approach Download PDFInfo
- Publication number
- CN107151278A CN107151278A CN201710280530.XA CN201710280530A CN107151278A CN 107151278 A CN107151278 A CN 107151278A CN 201710280530 A CN201710280530 A CN 201710280530A CN 107151278 A CN107151278 A CN 107151278A
- Authority
- CN
- China
- Prior art keywords
- corvic
- post
- organic phase
- organic solvent
- mentioned
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/008—Treatment of solid polymer wetted by water or organic solvents, e.g. coagulum, filter cakes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/02—Neutralisation of the polymerisation mass, e.g. killing the catalyst also removal of catalyst residues
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)
Abstract
The invention provides a kind of Corvic post-processing approach, including following seven specific steps：Addition alcohol organic solvent is filtrated to get filter cake, filter cake and is dissolved in addition saturated aqueous common salt extraction in organic solvent, organic phase, decolourizes, be dehydrated, depressurizing removal of impurities and drying, obtains the high polyvinyl chloride product of purity；Compared with prior art, the present invention has advantages below：By using multiple process for refining, it can effectively remove and hydrogen chloride and many alkenes low-boiling-point organic compound matter because of pyrolytic generation are produced in metal water-solubility impurity, organic-inorganic pigment, moisture, residual organic solvent, the courses of reaction such as mechanical admixture, the polyvinyl chloride particles of coking such as the plasticizing piece of azo-initiator, agitator, the iron ion brought into by raw material vinyl chloride, the final polyvinyl chloride product purity of gained is high, it is specious, uniform granularity, good fluidity, no bad smell；The post-processing approach is easy to operate, reasonable in design in a word, is with a wide range of applications.
Description
Technical field
The present invention relates to polyvinyl chloride technical field of purification, and in particular to a kind of Corvic post-processing approach.
Background technology
Polyvinyl chloride, English abbreviation PVC is the polymerization that VCM is polymerized according to mechanism of free-radical polymerization
Thing, is the white powder of impalpable structure, and the degree of branching is smaller, relative density 1.4 or so, 77-90 DEG C of glass transition temperature, to light and
The stability of heat is poor, and stabilizer is must be added in actual applications to improve the stability to light and heat.Industrial PVC points
Son amount is general, and with larger polydispersity, and the reduction of molecular weight with polymerisation temperature increases in the range of 50,000-11 ten thousand, without solid
Determine fusing point, 80-85 DEG C starts softening, and 130 DEG C are changed into viscoelastic state, and 160-180 DEG C starts to be changed into viscous state, there is preferable machinery
Performance, tensile strength 60MPa or so, impact strength 5-10kJ/m2 has excellent dielectric properties.PVC was once that yield is most in the world
Big general-purpose plastics, using widely, in construction material, industrial product, commodity, flooring laminate, floor tile, artificial leather, pipe
It is widely used in terms of material, electric wire, packaging film, bottle, expanded material, encapsulant, fiber.
Polyvinyl chloride synthetic method has suspension polymerization, emulsion polymerization and mass polymerization.In the prior art because raw material,
Auxiliary agent, solvent purity are low, or the reason such as post-processing approach is incorrect, easily make to be mingled with various nothings in final polyvinyl chloride product
Machine and organic impurities, cause that product purity is low, shade deviation, and rough surface has bad smell, Quality Down, every physical mechanical
Performance indications are unsatisfactory for requirement, have a strong impact on its application.
Therefore, the problem how is solved, it has also become those skilled in the art's technical barrier urgently to be resolved hurrily.
The content of the invention
The present invention, there is provided a kind of Corvic post-processing approach, is solved for the deficiencies in the prior art
Above-mentioned technical problem.
To achieve these goals, the present invention provides following technical scheme：A kind of Corvic post-processing approach, bag
Include following specific steps：
（1）, first toward alcohol organic solvent is added in Corvic crude product, filtered after stirring, collection filter cake, except uncoupling
Nitrogen class initiator；
（2）, above-mentioned filter cake is added in the organic solvent of dissolvable polyvinyl chloride, be filtered to remove insoluble granule impurity, receive
Collect filtrate；
（3）, extract 2-3 time toward adding saturated aqueous common salt in above-mentioned filtrate, remove water-solubility impurity, collection organic phase；
（4）, boil 0.5-1h toward adding under adsorption decolouriser, counterflow condition in above-mentioned organic phase, be filtered to remove decolorising agent, collect
Organic phase after decolouring；
（5）, will add inorganic drying agents in the organic phase after above-mentioned decolouring, stand 0.5-2h, be filtered to remove drier, collect de-
Organic phase after water；
（6）, by the organic phase after above-mentioned dehydration vacuum be -0.1 to -0.6MPa, heating-up temperature be 40-55 DEG C under conditions of
Vacuum distillation is carried out, organic solvent and low-boiling-point organic compound matter is removed, bottoms are collected；
（7）, above-mentioned bottoms are put in drum-type drying case in 65-75 DEG C of dry 2-3h, the polyvinyl chloride purified
Product.
As a further improvement on the present invention, the step（1）In alcohol organic solvent be methanol or ethanol, can be with molten
Solve and remove azodiisobutyronitrile, AMBN, ABVN, azo-bis-isobutyrate hydrochloride, the hexamethylene of azo two
The azo-initiators such as base formonitrile HCN, and it is insoluble to polyvinyl chloride.
As a further improvement on the present invention, the step（2）In organic solvent be selected from cyclohexanone, dichloroethanes and four
One or more in hydrogen furans, can dissolve polyvinyl chloride, and plasticizing piece, coking to some mechanical admixtures such as agitator
Polyvinyl chloride particles do not dissolve, so that they be effectively separated, make product surface smoothness and purity higher, no stain
Spot.
Above-mentioned steps（3）Middle addition saturated aqueous common salt contributes to extracting and demixing, prevents from forming middle emulsion layer, while can remove
Go iron ion brought into by raw material vinyl chloride etc. to easily cause product colour flavescence and become auburn inorganic impurity.
As a further improvement on the present invention, the step（4）In adsorption decolouriser be selected from activated carbon, porous ceramics
One or more in grain, can adsorb inorganic and organic impurities, make the color of product more shallow whiter, no bad smell.
As a further improvement on the present invention, the step（5）In inorganic drying agents be selected from anhydrous sodium sulfate, anhydrous sulphur
One kind in sour magnesium, water absorption rate is high, and drier is quicksand like, convenient filtering.
Above-mentioned steps（6）Middle vacuum distillation, the alcohol organic solvent remained before can removing in operating process, for molten
Solve the organic solvent of polyvinyl chloride, and low-boiling point material, the hydrogen chloride gas produced in polymerization process etc..
Compared with prior art, the present invention has advantages below：Add by using following multiple process for refining, including successively
Enter alcohol organic solvent be filtrated to get filter cake, filter cake be dissolved in organic solvent, organic phase add saturated aqueous common salt extraction, it is de-
Color, dehydration, decompression removal of impurities and dry totally seven step, can effectively remove the machinery such as plasticizing piece of azo-initiator, agitator miscellaneous
The metal water-solubility impurity such as matter, the polyvinyl chloride particles of coking, the iron ion brought into by raw material vinyl chloride, organic-inorganic pigment,
Hydrogen chloride and many alkenes low-boiling-point organic compound matter because of pyrolytic generation are produced in moisture, residual organic solvent, course of reaction,
The final polyvinyl chloride product purity of gained is high, specious, uniform granularity, good fluidity, no bad smell；The rear place in a word
Reason method is easy to operate, reasonable in design, is with a wide range of applications.
Embodiment
With reference to specific embodiment, the present invention is expanded on further, it should be appreciated that these embodiments are merely to illustrate the present invention
Rather than limitation the scope of the present invention；In addition, it is to be understood that after present disclosure has been read, those skilled in the art can
To be made various changes or modifications to the present invention, these equivalent form of values also fall within appended claims limited range.
Embodiment 1
A kind of Corvic post-processing approach, is comprised the following specific steps that：
（1）, first toward 20L methanol organic solvents are added in 10Kg Corvic crude products, filtered after stirring, collect and filter
Cake, removes azo-initiator；
（2）, above-mentioned filter cake is added in the cyclohexanone solvent that 30L can dissolve polyvinyl chloride, be filtered to remove insoluble granule miscellaneous
Matter, collects filtrate；
（3）, extract 2 times toward adding saturated aqueous common salt in above-mentioned filtrate, 35L is added for the first time, 15L is added second, water is removed
Solubility impurity, collects organic phase；
（4）, boil 0.5h toward adding in above-mentioned organic phase under 50g adsorption decolouriser activated carbons, counterflow condition, be filtered to remove decolouring
Agent, collects the organic phase after decolourizing；
（5）, will in the organic phase after above-mentioned decolouring add 200g inorganic drying agents anhydrous sodium sulfates, stand 0.5h, be filtered to remove
Drier, collects the organic phase after dehydration；
（6）, by the organic phase after above-mentioned dehydration vacuum be -0.1MPa, heating-up temperature be 40 DEG C under conditions of depressurized
Distillation, removes organic solvent and low-boiling-point organic compound matter, collects bottoms；
（7）, above-mentioned bottoms are put in drum-type drying case in 65 DEG C of dry 2h, the white polyvinyl chloride production purified
Product.
Embodiment 2
A kind of Corvic post-processing approach, is comprised the following specific steps that：
（1）, first toward 20L ethanol organic solvents are added in 10Kg Corvic crude products, filtered after stirring, collect and filter
Cake, removes azo-initiator；
（2）, above-mentioned filter cake is added in the tetrahydrofuran solvent that 30L can dissolve polyvinyl chloride, be filtered to remove insoluble granule
Impurity, collects filtrate；
（3）, extract 3 times toward adding saturated aqueous common salt in above-mentioned filtrate, 35L is added for the first time, 15L is added second, water is removed
Solubility impurity, collects organic phase；
（4）, boil 0.75h toward adding in above-mentioned organic phase under 50g adsorption decolouriser porous ceramic particles, counterflow condition, filter
Decolorising agent is removed, the organic phase after decolourizing is collected；
（5）, will in the organic phase after above-mentioned decolouring add 200g inorganic drying agents anhydrous magnesium sulfates, stand 1h, be filtered to remove dry
Drying prescription, collects the organic phase after dehydration；
（6）, by the organic phase after above-mentioned dehydration vacuum be -0.6MPa, heating-up temperature be 48 DEG C under conditions of depressurized
Distillation, removes organic solvent and low-boiling-point organic compound matter, collects bottoms；
（7）, above-mentioned bottoms are put in drum-type drying case in 70 DEG C of dry 2.5h, the white polyvinyl chloride purified
Product.
Embodiment 3
A kind of Corvic post-processing approach, is comprised the following specific steps that：
（1）, first toward 20L methanol organic solvents are added in 10Kg Corvic crude products, filtered after stirring, collect and filter
Cake, removes azo-initiator；
（2）, will in above-mentioned filter cake add can dissolve polyvinyl chloride 20L cyclohexanone and 10L dichloroethanes formation mixed solvent,
Insoluble granule impurity is filtered to remove, filtrate is collected；
（3）, extract 2 times toward adding saturated aqueous common salt in above-mentioned filtrate, 35L is added for the first time, 15L is added second, water is removed
Solubility impurity, collects organic phase；
（4）, boiled under adsorption decolouriser 30g activated carbons and 20g porous ceramic particles, counterflow condition toward adding in above-mentioned organic phase
1h, is filtered to remove decolorising agent, collects the organic phase after decolourizing；
（5）, will in the organic phase after above-mentioned decolouring add 500g inorganic drying agents anhydrous sodium sulfates, stand 2h, be filtered to remove dry
Drying prescription, collects the organic phase after dehydration；
（6）, by the organic phase after above-mentioned dehydration vacuum be -0.3MPa, heating-up temperature be 55 DEG C under conditions of depressurized
Distillation, removes organic solvent and low-boiling-point organic compound matter, collects bottoms；
（7）, above-mentioned bottoms are put in drum-type drying case in 75 DEG C of dry 3h, the white polyvinyl chloride production purified
Product.
Claims (5)
1. a kind of Corvic post-processing approach, it is characterised in that comprise the following specific steps that：
（1）, first toward alcohol organic solvent is added in Corvic crude product, filtered after stirring, collection filter cake, except uncoupling
Nitrogen class initiator；
（2）, above-mentioned filter cake is added in the organic solvent of dissolvable polyvinyl chloride, be filtered to remove insoluble granule impurity, receive
Collect filtrate；
（3）, extract 2-3 time toward adding saturated aqueous common salt in above-mentioned filtrate, remove water-solubility impurity, collection organic phase；
（4）, boil 0.5-1h toward adding under adsorption decolouriser, counterflow condition in above-mentioned organic phase, be filtered to remove decolorising agent, collect
Organic phase after decolouring；
（5）, will add inorganic drying agents in the organic phase after above-mentioned decolouring, stand 0.5-2h, be filtered to remove drier, collect de-
Organic phase after water；
（6）, by the organic phase after above-mentioned dehydration vacuum be -0.1 to -0.6MPa, heating-up temperature be 40-55 DEG C under conditions of
Vacuum distillation is carried out, organic solvent and low-boiling-point organic compound matter is removed, bottoms are collected；
（7）, above-mentioned bottoms are put in drum-type drying case in 65-75 DEG C of dry 2-3h, the polyvinyl chloride purified
Product.
2. a kind of Corvic post-processing approach according to claim 1, it is characterised in that：The step（1）In
Alcohol organic solvent be methanol or ethanol.
3. a kind of Corvic post-processing approach according to claim 1, it is characterised in that：The step（2）In
One or more of the organic solvent in cyclohexanone, dichloroethanes and tetrahydrofuran.
4. a kind of Corvic post-processing approach according to claim 1, it is characterised in that：The step（4）In
One or more of the adsorption decolouriser in activated carbon, porous ceramic particles.
5. a kind of Corvic post-processing approach according to claim 1, it is characterised in that：The step（5）In
One kind in anhydrous sodium sulfate, anhydrous magnesium sulfate of inorganic drying agents.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710280530.XA CN107151278A (en) | 2017-04-26 | 2017-04-26 | A kind of Corvic post-processing approach |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710280530.XA CN107151278A (en) | 2017-04-26 | 2017-04-26 | A kind of Corvic post-processing approach |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107151278A true CN107151278A (en) | 2017-09-12 |
Family
ID=59792529
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710280530.XA Pending CN107151278A (en) | 2017-04-26 | 2017-04-26 | A kind of Corvic post-processing approach |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107151278A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE854224A (en) * | 1976-06-11 | 1977-11-03 | Basf Ag | PROCESS FOR TREATING SOLUTIONS OF POLYMRIZED VINYL CHLORIDE IN TETRAHYDROFURAN |
| CN1178977C (en) * | 1999-09-24 | 2004-12-08 | 索尔维公司 | Method for recycling vinyl polymer-based articles |
| CN1890296A (en) * | 2003-12-16 | 2007-01-03 | 杜邦电子聚合物公司 | Polymer purification |
| CN101061165A (en) * | 2004-11-22 | 2007-10-24 | 索维公司 | Process for the purification of vinyl chloride polymers (pvc) from heavy metals |
| CN102731785A (en) * | 2012-06-11 | 2012-10-17 | 张家港市新盛新材料有限公司 | Polyphenylene sulfide purifying method |
-
2017
- 2017-04-26 CN CN201710280530.XA patent/CN107151278A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| BE854224A (en) * | 1976-06-11 | 1977-11-03 | Basf Ag | PROCESS FOR TREATING SOLUTIONS OF POLYMRIZED VINYL CHLORIDE IN TETRAHYDROFURAN |
| CN1178977C (en) * | 1999-09-24 | 2004-12-08 | 索尔维公司 | Method for recycling vinyl polymer-based articles |
| CN1890296A (en) * | 2003-12-16 | 2007-01-03 | 杜邦电子聚合物公司 | Polymer purification |
| CN101061165A (en) * | 2004-11-22 | 2007-10-24 | 索维公司 | Process for the purification of vinyl chloride polymers (pvc) from heavy metals |
| CN102731785A (en) * | 2012-06-11 | 2012-10-17 | 张家港市新盛新材料有限公司 | Polyphenylene sulfide purifying method |
Non-Patent Citations (1)
| Title |
|---|
| E.A.柯林斯等著，王盈康等译: "《聚合物科学实验》", 30 September 1983, 科学出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104017205B (en) | Method for regenerating nylon | |
| CN107311205B (en) | The method for purifying potassium nitrate in tempered glass waste liquid | |
| CN110590746A (en) | Preparation method of low-impurity vonoprazan fumarate | |
| CN106395862B (en) | The recovery method of byproduct sodium chloride in a kind of polyphenylene sulfide production process | |
| CN101565189A (en) | Method for preparing sodium chloride and potassium chloride by using brine | |
| CN113083253B (en) | Weak acid cation resin for extracting vitamin B12 and synthetic method thereof | |
| CN105348422B (en) | A kind of preparation method of abietyl acrylamide polymer | |
| CN107151278A (en) | A kind of Corvic post-processing approach | |
| JP2021505366A (en) | Method of separating unreacted monomer from a mixed solution containing unreacted monomer | |
| CN109503382A (en) | A kind of 12 benzocyclobutene dehydroabietic acids (Beta-methyl acryloyl-oxyethyl) ester, preparation method and its applications | |
| CN112897599A (en) | Crystallization method of nickel sulfate, cobalt sulfate and manganese sulfate | |
| JP2000509320A (en) | Separation method of organic monomer or auxiliary agent | |
| CN102796262A (en) | Method for preparing sevelamer carbonate | |
| CN106380601A (en) | Purifying method for polyphenylene sulfide with high molecular weight | |
| CN109867739B (en) | Preparation method of brominated polystyrene | |
| CN109573975A (en) | A kind of extracting process of hydrochloric acid method phosphoric acid by wet process preparation high-quality phosphoric acid | |
| CN102382044A (en) | Purification method for 2,3-dimethylpyridine | |
| CN104974051A (en) | Synthetic method for (1S,4R)-cis-4-amino-2-cyclopentene-1-methanol hydrochloride | |
| CN107936288A (en) | A kind of method of NMP and LiCl in the recycling polyphenylene sulfide production by solvent extraction process technology | |
| CN107973760A (en) | The method for preparing epoxychloropropane | |
| CN110563869B (en) | Resin type polypeptide condensation reagent and preparation method and application thereof | |
| DE2402697A1 (en) | CROSS-LINKED POLYMERIC RESIN AND METHOD FOR MANUFACTURING IT | |
| CN107501553A (en) | A kind of preparation method of the polyphenylene sulfide of no catalyst | |
| CN101693644B (en) | Process for preparing high heat stability decabromdiphenylethane | |
| CN110669229A (en) | Dynamic imine macrocycle-based supramolecular polymer and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170912 |