CN109912384A - A kind of catalysis process recycling dichloropropylene from dichloropropylene polymer - Google Patents
A kind of catalysis process recycling dichloropropylene from dichloropropylene polymer Download PDFInfo
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- CN109912384A CN109912384A CN201910273314.1A CN201910273314A CN109912384A CN 109912384 A CN109912384 A CN 109912384A CN 201910273314 A CN201910273314 A CN 201910273314A CN 109912384 A CN109912384 A CN 109912384A
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- dichloropropylene
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- dimethylformamide
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Abstract
The invention discloses a kind of from dichloropropylene polymer recycles the catalysis process of dichloropropylene.Step includes: to add dichloropropylene polymer, N,N-dimethylformamide, catalyst in the reaction vessel；The dosage of n,N-Dimethylformamide is 5 ~ 30 times of poly body weight, and the dosage of catalyst is 0.1 ~ 1 times of poly body weight；After addition, 3 ~ 9h is reacted at 20 ~ 80 DEG C；After reaction, reaction system is rotated, isolates dichloropropylene.The method that the present invention recycles dichloropropylene from dichloropropylene polymer, be it is a kind of it is easy to operate, process is short, product is easily separated, production process is without discharge, safety and environmental protection, low cost, and the industrial method being easily achieved.
Description
Technical field
The present invention relates to a kind of from dichloropropylene polymer recycles the catalysis process of dichloropropylene.The present invention relates to one kind
Make the breaking of covalent bonds of polymer using chemical method, the method for realizing dichloropropylene recycling is a kind of easy to operate, process
It is short, product is easily separated, production process is without discharge, safety and environmental protection, low cost, and the industrial method being easily achieved, be mainly used for
Chemical plant.
Background technique
Dichloropropylene polymer is usually the by-product generated in certain production workshop sections, such as the production work of the ether of oxime containing chlorine
Section is done solid waste processing mostly and is directly abandoned.Chlorine-containing waste can cause environmental pollution, and present invention consideration is carried out depolymerization
It at monomer and recycles, is greatly improved the utilization rate of dichloropropylene, reduce production cost.
Summary of the invention
In order to solve the problems, such as the processing of chlorine-containing waste, the object of the present invention is to provide one kind from dichloropropylene polymer
Recycle the catalysis process of dichloropropylene.
A kind of catalysis process recycling dichloropropylene from dichloropropylene polymer, step include:
(1) dichloropropylene polymer, N,N-dimethylformamide, catalyst is added into reactor at room temperature；N, N- diformazan
The quality of base formamide is 5 ~ 30 times of multimer mass, and the quality of catalyst is 0.1 ~ 1 times of multimer mass；
(2) temperature is raised to 20 ~ 80 DEG C, stirred, 3 ~ 10h of insulation reaction；
(3) reaction system is rotated, collects the dichloropropylene isolated.
Catalyst in the step (1) is azochlorosulfonate acid resin catalyst.
The quality of N,N-dimethylformamide is 10 ~ 20 times of dichloropropylene multimer mass in the step (1).
The dosage of catalyst is 0.1 ~ 0.5 times of poly body weight in the step (1).
Reaction temperature is 25 ~ 75 DEG C in the step (2), and the reaction time is 6 ~ 9h.
In the step (3), revolving temperature is 70 DEG C.
The production workshop section of dichloropropylene polymer in the step (1) from the ether of oxime containing chlorine.
The beneficial effects of the present invention are:
1) this method can effectively be recycled dichloropropylene by shirtsleeve operation from polymer；
2) temperature 70 C is rotated in method, solvent can be separated from reaction system and prevented to product dichloropropylene
N,N-dimethylformamide evaporation.
Detailed description of the invention
Fig. 1 is the gas chromatography-mass spectrum figure (having removed solvent peak) of dichloroethylene polymer before reacting, and upper half is gas phase
Chromatogram, lower half are the mass spectrograms at 5.184min；
Fig. 2 is the gas chromatography-mass spectrum figure (having removed solvent peak) of dichloroethylene polymer after reacting 9h, and upper half is gas phase color
Spectrogram, lower half are the mass spectrograms at 5.200min；
Fig. 3 is the content of each component in dichloroethylene polymer before reacting；
Fig. 4 is the content of each component in dichloroethylene polymer after reacting 9h.
Specific embodiment
Below in conjunction with drawings and examples, the present invention is further elaborated.
Embodiment 1
(1) 1.2912g dichloropropylene is added into the 50mL flask that magnetic stirring apparatus, thermometer, condenser pipe are housed at room temperature
Polymer, 20mL N,N-dimethylformamide, 0.3376g azochlorosulfonate acid resin catalyst；
The sample before answering is negated, gas chromatography-mass spectrometry analysis is carried out, as shown in Figure 1, the mass spectrogram at 5.184 shows the peak institute
Corresponding substance, molecular mass 112 are dichloropropylene.
As shown in figure 3, the corresponding peak area in 5.184 places accounts for 27.34%, that is, the mass fraction of dichloropropylene is before reacting
27.34%。
(2) reaction temperature is raised to 75 DEG C, starts magnetic stirring apparatus, insulation reaction 9h；
The sample after answering is negated, gas chromatography-mass spectrometry analysis is carried out, discovery has product generation.As shown in Fig. 2, the matter at 5.200
Spectrogram shows substance corresponding to the peak, and molecular mass 112 is dichloropropylene.
As shown in figure 4, the corresponding peak area in 5.200 places accounts for 73.94%, that is, the mass fraction of dichloropropylene is after reacting
73.94%。
(3) after reaction, reaction system is rotated at 70 DEG C, collects the dichloropropylene isolated, product is received
Rate 70.1%, purity 99.0%.
Comparative example 1
(1) 1.2875g dichloropropylene is added into the 50mL flask that magnetic stirring apparatus, thermometer, condenser pipe are housed at room temperature
Polymer, 20mL N,N-dimethylformamide, 0.3389g azochlorosulfonate acid resin catalyst；
(2) reaction temperature is raised to 25 DEG C, starts magnetic stirring apparatus, insulation reaction 9h；
The sample before answering and after reaction is negated, carries out gas chromatography-mass spectrometry analysis, there is no products to generate for discovery.
Comparative example 2
(1) 1.2909g dichloropropylene is added into the 50mL flask that magnetic stirring apparatus, thermometer, condenser pipe are housed at room temperature
Polymer, 20mL N,N-dimethylformamide, 0.3400g azochlorosulfonate acid resin catalyst；
(2) reaction temperature is raised to 50 DEG C, starts magnetic stirring apparatus, insulation reaction 9h；
The sample before answering and after reaction is negated, carries out gas chromatography-mass spectrometry analysis, there is no products to generate for discovery.
Claims (7)
1. a kind of catalysis process for recycling dichloropropylene from dichloropropylene polymer, which is characterized in that its step includes:
(1) dichloropropylene polymer, N,N-dimethylformamide, catalyst is added into reactor at room temperature；N, N- diformazan
The quality of base formamide is 5 ~ 30 times of multimer mass, and the quality of catalyst is 0.1 ~ 1 times of multimer mass；
(2) temperature is raised to 20 ~ 80 DEG C, stirred, 3 ~ 10h of insulation reaction；
(3) reaction system is rotated, collects the dichloropropylene isolated.
2. the method according to claim 1, wherein the catalyst in the step (1) is sulfonate resin catalysis
Agent.
3. the method according to claim 1, wherein in the step (1) n,N-Dimethylformamide quality
It is 10 ~ 20 times of dichloropropylene multimer mass.
4. the method according to claim 1, wherein the dosage of catalyst is poly weight in the step (1)
0.1 ~ 0.5 times of amount.
5. being reacted the method according to claim 1, wherein reaction temperature is 25 ~ 75 DEG C in the step (2)
Time is 6 ~ 9h.
6. the method according to claim 1, wherein revolving temperature is 70 DEG C in the step (3).
7. the method according to claim 1, wherein dichloropropylene polymer in the step (1) from
The production workshop section of the ether of oxime containing chlorine.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910273314.1A CN109912384A (en) | 2019-04-04 | 2019-04-04 | A kind of catalysis process recycling dichloropropylene from dichloropropylene polymer |
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| CN201910273314.1A CN109912384A (en) | 2019-04-04 | 2019-04-04 | A kind of catalysis process recycling dichloropropylene from dichloropropylene polymer |
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Citations (7)
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|---|---|---|---|---|
| US2588867A (en) * | 1948-10-25 | 1952-03-11 | Dow Chemical Co | Pyrolytic production of chlorohydrocarbons |
| US2664449A (en) * | 1947-01-06 | 1953-12-29 | William T Miller | Pyrolysis of trifluorochloroethylene polymers |
| CN1398839A (en) * | 2002-08-19 | 2003-02-26 | 中国石化长城润滑油集团有限公司 | Plant and process of cracking polytetrafluoroethylene to prepare tetrafluoroethylene monomer |
| CN1634818A (en) * | 2004-09-30 | 2005-07-06 | 南京博臣农化有限公司 | Process for preparing 2,3-dichloropropylene |
| CN101462925A (en) * | 2009-01-14 | 2009-06-24 | 中化国际（苏州）新材料研发有限公司 | Method for preparing tetrafluoroethylene by thermal cracking polytetrafluorethylene |
| CN102216246A (en) * | 2008-10-01 | 2011-10-12 | 3M创新有限公司 | Process of making fluoroolefins by thermal decomposition of fluorinated materials |
| CN104387226A (en) * | 2014-11-20 | 2015-03-04 | 闾正军 | Purification method of dichloropropene |
-
2019
- 2019-04-04 CN CN201910273314.1A patent/CN109912384A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2664449A (en) * | 1947-01-06 | 1953-12-29 | William T Miller | Pyrolysis of trifluorochloroethylene polymers |
| US2588867A (en) * | 1948-10-25 | 1952-03-11 | Dow Chemical Co | Pyrolytic production of chlorohydrocarbons |
| CN1398839A (en) * | 2002-08-19 | 2003-02-26 | 中国石化长城润滑油集团有限公司 | Plant and process of cracking polytetrafluoroethylene to prepare tetrafluoroethylene monomer |
| CN1634818A (en) * | 2004-09-30 | 2005-07-06 | 南京博臣农化有限公司 | Process for preparing 2,3-dichloropropylene |
| CN102216246A (en) * | 2008-10-01 | 2011-10-12 | 3M创新有限公司 | Process of making fluoroolefins by thermal decomposition of fluorinated materials |
| CN101462925A (en) * | 2009-01-14 | 2009-06-24 | 中化国际（苏州）新材料研发有限公司 | Method for preparing tetrafluoroethylene by thermal cracking polytetrafluorethylene |
| CN104387226A (en) * | 2014-11-20 | 2015-03-04 | 闾正军 | Purification method of dichloropropene |
Non-Patent Citations (4)
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| CHAO TANG ET AL.: "Catalytic effect of Al–Zn composite catalyst on the degradation of PVC-containing polymer mixtures into pyrolysis oil", 《POLYMER DEGRADATION AND STABILITY》 * |
| 伍艳辉等: "废塑料裂解催化剂研究进展", 《工业催化》 * |
| 周茜: "聚烯烃催化裂解产物控制与机理研究", 《中国博士学位论文全文数据库 工程科技Ⅰ辑》 * |
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