CN1100342A - Preparing method and use of catalyst for oriented chlorination of toluene - Google Patents
Preparing method and use of catalyst for oriented chlorination of toluene Download PDFInfo
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- CN1100342A CN1100342A CN 93115504 CN93115504A CN1100342A CN 1100342 A CN1100342 A CN 1100342A CN 93115504 CN93115504 CN 93115504 CN 93115504 A CN93115504 A CN 93115504A CN 1100342 A CN1100342 A CN 1100342A
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- Prior art keywords
- toluene
- catalyst
- chlorination
- chlorine
- reaction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C47/00—Compounds having —CHO groups
- C07C47/02—Saturated compounds having —CHO groups bound to acyclic carbon atoms or to hydrogen
- C07C47/14—Saturated compounds having —CHO groups bound to acyclic carbon atoms or to hydrogen containing halogen
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Catalysts (AREA)
Abstract
The catalyst is prepared with methylbenzyl chloride, sulphur dichloride, liquid chlorine and ferric trichloride as material and at the throw-in temp. of 50-60 deg.C and reaction-temp. of 70 minus or plus 2 deg.C for 6-8 hr. It is used in various equipment for the control of chlorination process resulting in methylbenzyl chloride, which has the freely adjustable ratio of orth- to para-methylbenzyl chloride, which has the freely adjustable ratio of roth- to paramethylbenzyl chloride in 0.85-1.40, the purity over 98%, the content of 2,4-dichloro methylbenzene below 0.5% and the raffinate after distillation below 3%.
Description
The present invention relates to the Manufacturing approach and use of catalyst for oriented chlorination of toluene, it belongs to formation or introduces the halogenating reaction class that contains heteroatom functional group.
In with the process of chlorination toluene method production-toluene(mono)chloride (tolyl chloride), use directional catalyst existing historical for many years, but generally all there is such-and-such problem, wherein comparatively distinct issues comprise: starting material have is difficult to obtain, manufacturing process is comparatively complicated, operability is undesirable, especially the value fluctuation range of ortho-chlorotolu'ene/parachlorotoluene is bigger in the product, and toluene dichloride and vinasse amount are also higher.
The purpose of this invention is to provide and a kind ofly make the method for described directional catalyst with the raw material that conveniently is easy to get, it in use has the advantage of easy handling, and face and directional effect are rather good.
The manufacture method of chlorination toluene directional catalyst of the present invention comprises: the raw material of employing has tolyl chloride (ortho-chlorotolu'ene or parachlorotoluene, purity 〉=98%) 100 weight parts, disulphur dichloride (sulfur monochloride, active chlorine content 50～53%) 3.5～5 weight parts, liquid chlorine (chlorinity 99.6%, V/V) 60～90 weight parts and FeCl3(purity 〉=96%, FeCl2≤2%, water-insoluble≤2%) 0.5～0.6 weight part.Preparation condition is: 50～60 ℃ of feed temperatures, and 2 hours, temperature of reaction 70 ± 20,10～12 hours, it was 1.220～1.250(d that liquid product proportion is surveyed in the reaction end of a period
20
4); The gained catalyst applications is: being used for chlorination toluene control-charge ratio according to following method on the intermittent type chloridizing unit is toluene: chlorine: chlorination toluene directional catalyst: promotor SbCl5(purity 〉=97%)=1: 0.6～0.7: 0.005～0.015: 0～0.0005,10～15 ℃ of temperature of reaction, 16～19 hours time, chlorine flux 60～80kg/h, catalyzer add indegree 3 times.On the continous way chloridizing unit, be used to control toluene chlorination-toluene flux 200～2501/h, chlorine flowrate 10～20m according to following condition
3/ h, (pressure 0.10～0.18MPa), the directional catalyst addition is 1% of a toluene consumption, is 25 ± 5 ℃ and the consumption of promotor SbCl5 is 0～0.05% temperature of reaction of toluene consumption.
Directional catalyst of the present invention is a kind of liquid, and the starting material source of making it is wide, and manufacture method is also uncomplicated, uses also easily, and the common laborer also can operate under a technician instructs.Use this catalyzer from toluene and chlorine production ortho-chlorotolu'ene, parachlorotoluene, transformation efficiency can reach 90%, and selectivity can reach more than 96%; Ortho-chlorotolu'ene and parachlorotoluene ratio are 0.85～1.40/1 in the product, and orientable adjusting, and wherein 2.4-toluene dichloride content is lower than 0.5%, distillation residual liquid amount＜3%; Gained neighbour, parachlorotoluene purity all are higher than 98% after rectifying separation.
Embodiment 1(Preparation of catalysts)
Get ortho-chlorotolu'ene 200kg, FeCl3 1.2kg, S2Cl2 10kg, logical chlorine dose 5m
3/ h, 50～60 ℃ of feed temperatures, 70 ± 2 ℃ of temperature of reaction; Should end gained liquid specific gravity d after 12 hours
20
4=1.250; The heavy 240kg of product.
Embodiment 2(Preparation of catalysts)
Get parachlorotoluene 200kg, FeCl3 1kg, S2Cl2 7kg, logical chlorine dose 8m
3/ h * 8h, temperature of reaction is with embodiment 1; Record liquid specific gravity d
20
4Stop logical chlorine after=1.220, get product 230kg.
Embodiment 3(Application of Catalyst)
In the enamel reaction still that band stirs, drop into toluene 1.5m
3, gained directional catalyst 13kg and the purity SbCl5 promotor 0.65kg more than 97% divides three addings among the embodiment 1,10～15 ℃ of temperature of reaction, and the logical chlorine total amount in 19 hours is 900kg; Products therefrom volume 1.6m
3, adjacency pair is than 0.86,2.4-toluene dichloride 0.4%, vinasse amount 1:10%.
Embodiment 4(Application of Catalyst)
On the continuous chlorination device, comply with following conditional operation: toluene flux 240 1/h, logical chlorine dose 19m
3/ h, 25 ± 5 ℃ of temperature of reaction, directional catalyst add-on are 1% of toluene add-on; Products therefrom proportion 1.080, adjacency pair are than 1.39, and the 2.4-toluene dichloride accounts for 0.38%, and the vinasse amount is 2.6% of a total amount.
Claims (2)
1, the manufacture method of catalyst for oriented chlorination of toluene is characterized in that:
(1) it be adopt following raw material-
(a) tolyl chloride (ortho-chlorotolu'ene or parachlorotoluene, its purity 〉=98%) 100 weight parts;
(b) disulphur dichloride (sulfur monochloride), (active chlorine content 50～53%) 3.5～5 weight parts;
(c) liquid chlorine (chlorinity 99.6%, V/V) 60～90 weight parts and (d) Fec13 (purity 〉=96%, Fecl2≤2%, water-insoluble≤2%) 0.5～0.6 weight part;
(2) comply with following condition to prepare-
(a) feed temperature is 50～60 ℃, and 2 hours,
(b) temperature of reaction is 70 ± 2 ℃, and 10～12 hours,
(c) reaction end of a period survey liquid product proportion is 1.220～1.250 (d
4 20).
2, the purposes of the described catalyst for oriented chlorination of toluene of claim 1 is characterized in that:
(1) on the intermittent type chloridizing unit, be used for chlorination toluene according to following method to control-
(a) charge ratio is a toluene: chlorine: catalyst for oriented chlorination: promotor sbcl5(content 〉=97%)=1: 0.6～0.7: 0.005～0.015: 0～0.0005,
(b) temperature of reaction is 10～15 ℃, 16～19 hours time,
(c) chlorine flux 60～80kg/h,
(d) catalyzer adds indegree, 3 times;
(2) on the continous way chloridizing unit according to following condition be used to control toluene chlorination-
(a) toluene flux 200～250l/h, chlorine flowrate 10～20M
3/ h(pressure 0.10～0.18MPa), the catalyst for oriented chlorination consumption is 0.5～1.5% of a toluene consumption, the consumption of promotor sbcl5 is 0～0.05% of a toluene consumption,
(b) temperature of reaction is 25 ± 5 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115504 CN1100342A (en) | 1993-09-14 | 1993-09-14 | Preparing method and use of catalyst for oriented chlorination of toluene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 93115504 CN1100342A (en) | 1993-09-14 | 1993-09-14 | Preparing method and use of catalyst for oriented chlorination of toluene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1100342A true CN1100342A (en) | 1995-03-22 |
Family
ID=4991079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 93115504 Pending CN1100342A (en) | 1993-09-14 | 1993-09-14 | Preparing method and use of catalyst for oriented chlorination of toluene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1100342A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102243A (en) * | 2013-03-08 | 2013-05-15 | 江苏超跃化学有限公司 | Method for preparing chlorotoluene |
| CN103910609A (en) * | 2014-04-10 | 2014-07-09 | 安徽海华科技股份有限公司 | Method for synthesizing cresol |
| CN108404828A (en) * | 2018-03-30 | 2018-08-17 | 北京万水净水剂有限公司 | A kind of process control method and reaction tower of ferric trichloride production process |
-
1993
- 1993-09-14 CN CN 93115504 patent/CN1100342A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103102243A (en) * | 2013-03-08 | 2013-05-15 | 江苏超跃化学有限公司 | Method for preparing chlorotoluene |
| CN103910609A (en) * | 2014-04-10 | 2014-07-09 | 安徽海华科技股份有限公司 | Method for synthesizing cresol |
| CN103910609B (en) * | 2014-04-10 | 2015-09-30 | 安徽海华科技股份有限公司 | A kind of synthetic method of cresols |
| CN108404828A (en) * | 2018-03-30 | 2018-08-17 | 北京万水净水剂有限公司 | A kind of process control method and reaction tower of ferric trichloride production process |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |