CN105037082A - Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor - Google Patents
Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor Download PDFInfo
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- CN105037082A CN105037082A CN201510313312.2A CN201510313312A CN105037082A CN 105037082 A CN105037082 A CN 105037082A CN 201510313312 A CN201510313312 A CN 201510313312A CN 105037082 A CN105037082 A CN 105037082A
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- santochlor
- mother liquor
- paradichlorobenzene
- polyphenylene sulfide
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Abstract
The invention discloses a method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor. The method comprises the following steps: (1) firstly filtering the polyphenylene sulphide production mother liquor and removing impurities; (2) distilling the filtered polyphenylene sulphide production mother liquor at the temperature of 150-200 DEG C, so that an NMP solvent and paradichlorobenzene waste water are obtained; (3) then settling the paradichlorobenzene waste water for 6-18 hours at the temperature of 0-30 DEG C; (4) centrifuging and separating settled paradichlorobenzene to obtain crude paradichlorobenzene crystals; (5) melting the crude paradichlorobenzene crystals at the temperature of 50-80 DEG C, so that liquid-state crude paradichlorobenzene is obtained; (6) filtering liquid-state crude paradichlorobenzene, and removing insoluble substances in liquid-state crude paradichlorobenzene; and (7) settling liquid-state paradichlorobenzene with the insoluble substances removed for 1-2 hours at the temperature of 0-20 DEG C, so that refined paradichlorobenzene crystals are obtained. The method disclosed by the invention has the advantage that paradichlorobenzene in the polyphenylene sulphide production mother liquor can be recycled.
Description
Technical field
The present invention relates to the recovery method that polyphenylene sulfide produces santochlor in mother liquor.
Background technology
Domestic and international production polyphenylene sulfide many employings sodium sulfide method, the raw material that sodium sulfide method uses is santochlor and sodium sulphite, the solvent used is N-Methyl pyrrolidone (being called for short NMP), raw material and solvent define polyphenylene sulfide reaction mother liquor, and in proportioning raw materials, the molar weight of santochlor generally need have more 1-10% than sodium sulphite.Produce in the process of polyphenylene sulfide at sodium sulfide method, sodium sulphite in polyphenylene sulfide reaction mother liquor and santochlor complete after polycondensation obtains polyphenylene sulfide, also want the polyphenylene sulfide in p-poly-phenyl thioether reaction mother liquor to carry out centrifugation and just can obtain polyphenylene sulfide product, in the polyphenylene sulfide reaction mother liquor after centrifugation, remain santochlor; Then the polyphenylene sulfide product to centrifugation obtains also is needed to wash, liquid after washing polyphenylene sulfide product is also referred to as polyphenylene sulfide product washings, also remain santochlor in polyphenylene sulfide product washings, polyphenylene sulfide product washings and centrifugal after polyphenylene sulfide reaction mother liquor define polyphenylene sulfide and produce mother liquor.After current sodium sulfide method produces polyphenylene sulfide, santochlor residual in mother liquor cannot be produced reclaim by p-poly-phenyl thioether, not only cause the waste of resource, and considerably increase enterprise's use cost, and because santochlor has benzene ring structure, polyphenylene sulfide is made to produce the biodegradability of mother liquor poor, and then very easily contaminate environment.
Summary of the invention
The object of this invention is to provide the santochlor recovery method that a kind of energy efficient recovery polyphenylene sulfide produces santochlor in mother liquor.
For achieving the above object, present invention employs following technical scheme: described polyphenylene sulfide produces the recovery method of santochlor in mother liquor, comprises the following steps:
(1) first p-poly-phenyl thioether production mother liquor filters, the oligopolymer in removing mixed solution;
(2) then the polyphenylene sulfide after filtration is produced mother liquor to distill under the temperature condition of 150 ~ 200 DEG C, obtain nmp solvent and santochlor waste water;
(3) then by santochlor waste water sedimentation 6 ~ 18h under the temperature condition of 0 ~ 30 DEG C;
(4) then centrifugation is carried out to the santochlor waste water after sedimentation and obtain thick santochlor crystallization;
(5) then thick santochlor crystallization is carried out melting under the temperature condition of 50 ~ 80 DEG C, form liquid thick santochlor;
(6) then the thick santochlor of liquid towards filters, the insolubles in the liquid thick santochlor of removing;
(7) then by the thick santochlor of liquid state sedimentation 1 ~ 2h under the temperature condition of 0 ~ 20 DEG C of removing insolubles, refining santochlor crystallization is obtained.
Further, aforesaid polyphenylene sulfide produces the recovery method of santochlor in mother liquor, wherein: the polyphenylene sulfide after filtration is produced mother liquor and distilled under the temperature condition of 160 DEG C, obtains nmp solvent and santochlor waste water.
Further, aforesaid polyphenylene sulfide produces the recovery method of santochlor in mother liquor, wherein: by santochlor waste water sedimentation 12h under the temperature condition of 10 DEG C.
Further, aforesaid polyphenylene sulfide produces the recovery method of santochlor in mother liquor, wherein: thick santochlor crystallization is carried out melting under the temperature condition of 55 DEG C, forms liquid thick santochlor.
Further, aforesaid polyphenylene sulfide produces the recovery method of santochlor in mother liquor, wherein: by the thick santochlor of liquid state sedimentation 1.5h under the temperature condition of 15 DEG C of removing insolubles, obtain refining santochlor crystallization.
By the enforcement of technique scheme, the invention has the beneficial effects as follows: energy p-poly-phenyl thioether is produced santochlor residual in mother liquor and carried out recycling, not only greatly reduce enterprise's production and application cost, and effectively reduce the content that polyphenylene sulfide produces santochlor in mother liquor, and then improve the biodegradability that polyphenylene sulfide produces mother liquor, reduce the intractability that polyphenylene sulfide produces mother liquor, effectively reduce polyphenylene sulfide and produce mother liquor to the pollution of environment.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment one
Polyphenylene sulfide produces the recovery method of santochlor in mother liquor, comprises the following steps:
(1) first p-poly-phenyl thioether production mother liquor filters, the oligopolymer in removing mixed solution;
(2) then the polyphenylene sulfide after filtration is produced mother liquor to distill under the temperature condition of 150 DEG C, obtain nmp solvent and santochlor waste water;
(3) then by santochlor waste water sedimentation 6h under the temperature condition of 0 DEG C;
(4) then centrifugation is carried out to the santochlor waste water after sedimentation and obtain thick santochlor crystallization;
(5) then thick santochlor crystallization is carried out melting under the temperature condition of 50 DEG C, form liquid thick santochlor;
(6) then the thick santochlor of liquid towards filters, the insolubles in the liquid thick santochlor of removing;
(7) then by the thick santochlor of liquid state sedimentation 1h under the temperature condition of 0 DEG C of removing insolubles, refining santochlor crystallization is obtained.
Embodiment two
Polyphenylene sulfide produces the recovery method of santochlor in mother liquor, comprises the following steps:
(1) first p-poly-phenyl thioether production mother liquor filters, the oligopolymer in removing mixed solution;
(2) then the polyphenylene sulfide after filtration is produced mother liquor to distill under the temperature condition of 160 DEG C, obtain nmp solvent and santochlor waste water;
(3) then by santochlor waste water sedimentation 12h under the temperature condition of 10 DEG C;
(4) then centrifugation is carried out to the santochlor waste water after sedimentation and obtain thick santochlor crystallization;
(5) then thick santochlor crystallization is carried out melting under the temperature condition of 55 DEG C, form liquid thick santochlor;
(6) then the thick santochlor of liquid towards filters, the insolubles in the liquid thick santochlor of removing;
(7) then by the thick santochlor of liquid state sedimentation 1.5h under the temperature condition of 15 DEG C of removing insolubles, refining santochlor crystallization is obtained.
Embodiment three
Polyphenylene sulfide produces the recovery method of santochlor in mother liquor, comprises the following steps:
(1) first p-poly-phenyl thioether production mother liquor filters, the oligopolymer in removing mixed solution;
(2) then the polyphenylene sulfide after filtration is produced mother liquor to distill under the temperature condition of 200 DEG C, obtain nmp solvent and santochlor waste water;
(3) then by santochlor waste water sedimentation 18h under the temperature condition of 30 DEG C;
(4) then centrifugation is carried out to the santochlor waste water after sedimentation and obtain thick santochlor crystallization;
(5) then thick santochlor crystallization is carried out melting under the temperature condition of 80 DEG C, form liquid thick santochlor;
(6) then the thick santochlor of liquid towards filters, the insolubles in the liquid thick santochlor of removing;
(7) then by the thick santochlor of liquid state sedimentation h under the temperature condition of 20 DEG C of removing insolubles, refining santochlor crystallization is obtained.
Advantage of the present invention is: energy p-poly-phenyl thioether is produced santochlor residual in mother liquor and carried out recycling, not only greatly reduce enterprise's production and application cost, and effectively reduce the content that polyphenylene sulfide produces santochlor in mother liquor, and then improve the biodegradability that polyphenylene sulfide produces mother liquor, reduce the intractability that polyphenylene sulfide produces mother liquor, effectively reduce polyphenylene sulfide and produce mother liquor to the pollution of environment.
Claims (5)
1. polyphenylene sulfide produces the recovery method of santochlor in mother liquor, it is characterized in that: comprise the following steps:
(1) first p-poly-phenyl thioether production mother liquor filters, the oligopolymer in removing mixed solution;
(2) then the polyphenylene sulfide after filtration is produced mother liquor to distill under the temperature condition of 150 ~ 200 DEG C, obtain nmp solvent and santochlor waste water;
(3) then by santochlor waste water sedimentation 6 ~ 18h under the temperature condition of 0 ~ 30 DEG C;
(4) then centrifugation is carried out to the santochlor waste water after sedimentation and obtain thick santochlor crystallization;
(5) then thick santochlor crystallization is carried out melting under the temperature condition of 50 ~ 80 DEG C, form liquid thick santochlor;
(6) then the thick santochlor of liquid towards filters, the insolubles in the liquid thick santochlor of removing;
(7) then by the thick santochlor of liquid state sedimentation 1 ~ 2h under the temperature condition of 0 ~ 20 DEG C of removing insolubles, refining santochlor crystallization is obtained.
2. polyphenylene sulfide according to claim 1 produces the recovery method of santochlor in mother liquor, it is characterized in that: the polyphenylene sulfide after filtration is produced mother liquor and distilled under the temperature condition of 160 DEG C, obtains nmp solvent and santochlor waste water.
3. polyphenylene sulfide according to claim 1 produces the recovery method of santochlor in mother liquor, it is characterized in that: by santochlor waste water sedimentation 12h under the temperature condition of 10 DEG C.
4. polyphenylene sulfide according to claim 1 produces the recovery method of santochlor in mother liquor, it is characterized in that: thick santochlor crystallization is carried out melting under the temperature condition of 55 DEG C, forms liquid thick santochlor.
5. polyphenylene sulfide according to claim 1 produces the recovery method of santochlor in mother liquor, it is characterized in that: by the thick santochlor of liquid state sedimentation 1.5h under the temperature condition of 15 DEG C of removing insolubles, obtain refining santochlor crystallization.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510313312.2A CN105037082A (en) | 2015-06-10 | 2015-06-10 | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510313312.2A CN105037082A (en) | 2015-06-10 | 2015-06-10 | Method for recycling paradichlorobenzene in polyphenylene sulphide production mother liquor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111620803A (en) * | 2020-05-11 | 2020-09-04 | 山东滨化滨阳燃化有限公司 | System and method for separating and recovering solvent and raw materials in polyphenylene sulfide production |
| CN112358096A (en) * | 2020-10-23 | 2021-02-12 | 重庆聚狮新材料科技有限公司 | Refining method for polyphenylene sulfide rectification recovered water |
| CN114539024A (en) * | 2022-03-09 | 2022-05-27 | 山东明化新材料有限公司 | Method for recovering p-dichlorobenzene in polyphenylene sulfide production process |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3658659A (en) * | 1969-09-24 | 1972-04-25 | Phillips Petroleum Co | Separating p-dichlorobenzene from n-methyl pyrrolidone by steam distillation |
| CN87104975A (en) * | 1986-07-17 | 1988-04-27 | 布雷克顿化学有限公司 | The method of purification santochlor |
| CN101492344A (en) * | 2008-11-04 | 2009-07-29 | 丹阳中超化工有限公司 | P-chlorotoluene purification process |
| JP2010144085A (en) * | 2008-12-19 | 2010-07-01 | Tosoh Corp | Process for producing polyphenylene sulfide |
| CN102675039A (en) * | 2012-06-11 | 2012-09-19 | 江苏隆昌化工有限公司 | Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials |
-
2015
- 2015-06-10 CN CN201510313312.2A patent/CN105037082A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3658659A (en) * | 1969-09-24 | 1972-04-25 | Phillips Petroleum Co | Separating p-dichlorobenzene from n-methyl pyrrolidone by steam distillation |
| CN87104975A (en) * | 1986-07-17 | 1988-04-27 | 布雷克顿化学有限公司 | The method of purification santochlor |
| CN101492344A (en) * | 2008-11-04 | 2009-07-29 | 丹阳中超化工有限公司 | P-chlorotoluene purification process |
| JP2010144085A (en) * | 2008-12-19 | 2010-07-01 | Tosoh Corp | Process for producing polyphenylene sulfide |
| CN102675039A (en) * | 2012-06-11 | 2012-09-19 | 江苏隆昌化工有限公司 | Process for producing m-dichlorobenzene by using chloridized aromatic hydrocarbon waste as raw materials |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111620803A (en) * | 2020-05-11 | 2020-09-04 | 山东滨化滨阳燃化有限公司 | System and method for separating and recovering solvent and raw materials in polyphenylene sulfide production |
| CN112358096A (en) * | 2020-10-23 | 2021-02-12 | 重庆聚狮新材料科技有限公司 | Refining method for polyphenylene sulfide rectification recovered water |
| CN114539024A (en) * | 2022-03-09 | 2022-05-27 | 山东明化新材料有限公司 | Method for recovering p-dichlorobenzene in polyphenylene sulfide production process |
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