CN102836731A - Catalyst used in preparation of paradichlorobenzene and method for preparing paradichlorobenzene by using such catalyst - Google Patents
Catalyst used in preparation of paradichlorobenzene and method for preparing paradichlorobenzene by using such catalyst Download PDFInfo
- Publication number
- CN102836731A CN102836731A CN2012103779691A CN201210377969A CN102836731A CN 102836731 A CN102836731 A CN 102836731A CN 2012103779691 A CN2012103779691 A CN 2012103779691A CN 201210377969 A CN201210377969 A CN 201210377969A CN 102836731 A CN102836731 A CN 102836731A
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- China
- Prior art keywords
- benzene
- catalyst
- paracide
- paradichlorobenzene
- ferric trichloride
- 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.)
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- OCJBOOLMMGQPQU-UHFFFAOYSA-N 1,4-dichlorobenzene Chemical compound ClC1=CC=C(Cl)C=C1 OCJBOOLMMGQPQU-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 239000003054 catalyst Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000000034 method Methods 0.000 title claims abstract description 14
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 21
- PXJJSXABGXMUSU-UHFFFAOYSA-N disulfur dichloride Chemical compound ClSSCl PXJJSXABGXMUSU-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 claims abstract description 9
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 66
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 6
- 229910052801 chlorine Inorganic materials 0.000 claims description 6
- 239000000460 chlorine Substances 0.000 claims description 6
- ZPQOPVIELGIULI-UHFFFAOYSA-N 1,3-dichlorobenzene Chemical compound ClC1=CC=CC(Cl)=C1 ZPQOPVIELGIULI-UHFFFAOYSA-N 0.000 claims description 3
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000013078 crystal Substances 0.000 claims description 3
- 150000004816 dichlorobenzenes Chemical class 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 238000003825 pressing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 239000003513 alkali Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 239000004734 Polyphenylene sulfide Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000002781 deodorant agent Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 229920006258 high performance thermoplastic Polymers 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
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Abstract
The invention discloses a catalyst used in preparation of paradichlorobenzene and a method for preparing the paradichlorobenzene by using such catalyst, wherein iron trichloride and disulfur dichloride are mixed according to a mass ratio of 5:3-12:7. The catalyst and the method have the advantages that the paradichlorobenzene is prepared by using the composite catalyst of the iron trichloride and the disulfur dichloride, the disulfur dichloride has an orientation effect, the productivity of the paradichlorobenzene is improved, the production of trichlorobenzene is inhibited, the conversion and the selectivity of the reaction are improved, the productivity of the paradichlorobenzene in chlorinated liquid is obviously improved, the purity of the prepared paradichlorobenzene product reaches up to 99.95 percent, washing and alkaline washing are not required during preparation, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to a kind of catalyst for preparing paracide, and with the method for this Preparation of Catalyst paracide.
Background technology
Paracide is the raw material of agricultural chemicals, medicine and dyestuff, can be used as mould inhibitor and space deodorant after making with extra care, and also is the raw material of producing novel high-performance thermoplastic resin polyphenylene sulfide.Single catalyst SbCl is used in existing paracide preparation
3Or SbCl
2, the paracide content in the chlorated liquid of producing has only 50%～52%, and trichloro-benzenes content is greater than 2%.Because single catalyst SbCl
3Or SbCl
2Have water-solublely, so this chlorated liquid must pass through washing and alkali cleaning removal catalyst wherein, and then freezing, crystallization, separation obtain paracide and o-dichlorohenzene product.The waste water that this preparation process produces is more, influences environment, and can't obtain highly purified paracide product.
Summary of the invention
Goal of the invention: to the problems referred to above, the object of the invention one provides a kind of catalyst for preparing paracide; Two provide the method for this Preparation of Catalyst paracide of a kind of usefulness, improve the production rate of paracide, avoid contaminated wastewater.
Technical scheme: a kind of catalyst for preparing paracide; By ferric trichloride and disulphur dichloride 5: 3～12: 7 proportionings of pressing mass ratio; Wherein to be dissolved in the content of benzene be mass content 1200～1500ppm to ferric trichloride, and the volume ratio of disulphur dichloride and benzene dissolving is 1: 5.
The method of the above-mentioned Preparation of Catalyst paracide of a kind of usefulness, this method may further comprise the steps:
(1), ferric trichloride is dissolved with benzene, obtain containing the benzene of ferric trichloride, the mass content of ferric trichloride is 1200～1500ppm;
(2), with the dissolving in 1: 5 by volume of disulphur dichloride and benzene, obtain containing the benzene of disulphur dichloride;
(3), the said benzene of ferric trichloride that contains is squeezed into A reactor with the speed of 1100～1300kg/h, the said benzene that contains disulphur dichloride with the speed of 2.5～3L/h; Speed feeding chlorine with 1100～1200kg/h reacts 60～70 ℃ of reaction temperatures; The A reactor overflow gets into second reactor, feeds chlorine with the speed of 1000～1100kg/h and reacts 60～70 ℃ of reaction temperatures;
(4), the chlorated liquid that obtains of step (3) removes catalyst after rectifying, obtain containing the mixed chlorinated liquid of dichloro-benzenes and trichloro-benzenes, get into crystal system again and purify and obtain purity and reach 99.95% paracide.
Contain Benzene Chloride 15%, paracide 63%, o-dichlorohenzene 20%, m-dichlorobenzene 0.5%, trichloro-benzenes in the chlorated liquid that step (3) obtains less than 1.5%, above content is the quality percentage composition.
Beneficial effect: compared with prior art, advantage of the present invention is to adopt the composite catalyst of ferric trichloride and disulphur dichloride to prepare paracide, and disulphur dichloride wherein has positioning action; Improve the growing amount of paracide, suppress the generation of trichloro-benzenes, improved the conversion ratio and the selectivity of reaction; Paracide growing amount in the chlorated liquid is significantly improved; The paracide product purity that makes is up to 99.95%, and should need not washing and alkali cleaning in the preparation process, reduced environmental pollution.
Description of drawings
Accompanying drawing is the process chart with Preparation of Catalyst paracide of the present invention.
The specific embodiment
Below in conjunction with accompanying drawing and specific embodiment; Further illustrate the present invention; Should understand these embodiment only be used to the present invention is described and be not used in the restriction scope of the present invention; After having read the present invention, those skilled in the art all fall within the application's accompanying claims institute restricted portion to the modification of the various equivalent form of values of the present invention.
A kind of catalyst for preparing paracide, by ferric trichloride and disulphur dichloride 5: 3～12: 7 proportionings of pressing mass ratio, wherein to be dissolved in the content of benzene be mass content 1200～1500ppm to ferric trichloride, the volume ratio of disulphur dichloride and benzene dissolving is 1: 5.
Shown in accompanying drawing, the method for the above-mentioned Preparation of Catalyst paracide of a kind of usefulness, this method may further comprise the steps:
(1), the preparation of ferric trichloride: benzene is squeezed into the catalyst dissolution groove, and groove completely back adds ferric trichloride, and the mass content of ferric trichloride is 1200～1500ppm in the control flume.
(2), the preparation of disulphur dichloride: with disulphur dichloride and benzene 1: 5 by volume in another catalyst dissolution groove kind dissolving.
(3), will contain the benzene of ferric trichloride and squeeze into A reactor with the speed of 2.5～3L/h with the speed of 1100～1300kg/h, the benzene that contains disulphur dichloride, feed chlorine with the speed of 1100～1200kg/h and react 60～70 ℃ of reaction temperatures; The A reactor overflow gets into second reactor, feeds chlorine with the speed of 1000～1100kg/h and reacts 60～70 ℃ of reaction temperatures.Contain Benzene Chloride 15%, paracide 63%, o-dichlorohenzene 20%, m-dichlorobenzene 0.5%, trichloro-benzenes less than 1.5% in the chlorated liquid that reaction obtains, above content is the quality percentage composition.
(4), the chlorated liquid that obtains of step (3) removes catalyst after rectifying, obtain containing the mixed chlorinated liquid of dichloro-benzenes and trichloro-benzenes, get into crystal system again and purify and obtain purity and reach 99.95% paracide.
Claims (3)
1. catalyst for preparing paracide; It is characterized in that: by ferric trichloride and disulphur dichloride 5: 3～12: 7 proportionings of pressing mass ratio; Wherein to be dissolved in the content of benzene be mass content 1200～1500ppm to ferric trichloride, and the volume ratio of disulphur dichloride and benzene dissolving is 1: 5.
2. method with the described Preparation of Catalyst paracide of claim 1 is characterized in that this method may further comprise the steps:
(1), ferric trichloride is dissolved with benzene, obtain containing the benzene of ferric trichloride, the mass content of ferric trichloride is 1200～1500ppm;
(2), with the dissolving in 1: 5 by volume of disulphur dichloride and benzene, obtain containing the benzene of disulphur dichloride;
(3), the said benzene of ferric trichloride that contains is squeezed into A reactor with the speed of 1100～1300kg/h, the said benzene that contains disulphur dichloride with the speed of 2.5～3L/h; Speed feeding chlorine with 1100～1200kg/h reacts 60～70 ℃ of reaction temperatures; The A reactor overflow gets into second reactor, feeds chlorine with the speed of 1000～1100kg/h and reacts 60～70 ℃ of reaction temperatures;
(4), the chlorated liquid that obtains of step (3) removes catalyst after rectifying, obtain containing the mixed chlorinated liquid of dichloro-benzenes and trichloro-benzenes, get into crystal system again and purify and obtain purity and reach 99.95% paracide.
3. the method for preparing paracide according to claim 2; It is characterized in that: contain Benzene Chloride 15%, paracide 63%, o-dichlorohenzene 20%, m-dichlorobenzene 0.5%, trichloro-benzenes in the chlorated liquid that step (3) obtains less than 1.5%, above content is the quality percentage composition.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103779691A CN102836731A (en) | 2012-10-08 | 2012-10-08 | Catalyst used in preparation of paradichlorobenzene and method for preparing paradichlorobenzene by using such catalyst |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103779691A CN102836731A (en) | 2012-10-08 | 2012-10-08 | Catalyst used in preparation of paradichlorobenzene and method for preparing paradichlorobenzene by using such catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102836731A true CN102836731A (en) | 2012-12-26 |
Family
ID=47364610
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|---|---|---|---|
| CN2012103779691A Pending CN102836731A (en) | 2012-10-08 | 2012-10-08 | Catalyst used in preparation of paradichlorobenzene and method for preparing paradichlorobenzene by using such catalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739441A (en) * | 2014-01-09 | 2014-04-23 | 东南大学 | Method for increasing proportion of paradichlorobenzene in benzene chlorination product |
| CN109774267A (en) * | 2019-03-22 | 2019-05-21 | 广州市帝东环保科技有限公司 | A kind of environmental-friendly construction material with long service life and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4727201A (en) * | 1986-07-07 | 1988-02-23 | Phillips Petroleum Company | Preparation of 1,4-dichlorobenzene |
| CN1678550A (en) * | 2002-09-04 | 2005-10-05 | 吴羽化学工业株式会社 | Method for producing p-dichlorobenzene |
| WO2007017900A2 (en) * | 2005-05-26 | 2007-02-15 | Sisir Kumar Mandal | Preparation of para dichlorobenzene from benzene or mono chlorobenzene |
-
2012
- 2012-10-08 CN CN2012103779691A patent/CN102836731A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4727201A (en) * | 1986-07-07 | 1988-02-23 | Phillips Petroleum Company | Preparation of 1,4-dichlorobenzene |
| CN1678550A (en) * | 2002-09-04 | 2005-10-05 | 吴羽化学工业株式会社 | Method for producing p-dichlorobenzene |
| WO2007017900A2 (en) * | 2005-05-26 | 2007-02-15 | Sisir Kumar Mandal | Preparation of para dichlorobenzene from benzene or mono chlorobenzene |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103739441A (en) * | 2014-01-09 | 2014-04-23 | 东南大学 | Method for increasing proportion of paradichlorobenzene in benzene chlorination product |
| CN109774267A (en) * | 2019-03-22 | 2019-05-21 | 广州市帝东环保科技有限公司 | A kind of environmental-friendly construction material with long service life and preparation method thereof |
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| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
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Application publication date: 20121226 |