CN1113907A - Technology for producing refined 2,4-trichloro-benzene - Google Patents
Technology for producing refined 2,4-trichloro-benzene Download PDFInfo
- Publication number
- CN1113907A CN1113907A CN 94106841 CN94106841A CN1113907A CN 1113907 A CN1113907 A CN 1113907A CN 94106841 CN94106841 CN 94106841 CN 94106841 A CN94106841 A CN 94106841A CN 1113907 A CN1113907 A CN 1113907A
- Authority
- CN
- China
- Prior art keywords
- trichlorobenzene
- crude product
- trichloro
- benzene
- product
- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C17/00—Preparation of halogenated hydrocarbons
- C07C17/38—Separation; Purification; Stabilisation; Use of additives
- C07C17/392—Separation; Purification; Stabilisation; Use of additives by crystallisation; Purification or separation of the crystals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The void substance of the lindane by-product is undergone the alkaline hydrolysis or pyrolysis then the mixed crude product of trichloro-benzene (containing 75% of 1,2,4-trichloro-benzene) is obtained after separation and dewatering, then the crude product is cooled to 20-30 deg.C, and crystallized under agitating with speed of 30-40 rpm and the crystalline temp. is maintained at 5-20 deg.C. After crystallization, the solid and liquid are separated and the active carbon or pottery clay filter is used to conduct the decolouring filtering, then the refined product over 99% content of 1,2,4-trichloro-benzene is obtained. The features of said technological method are small investment for equipment. Small raw material consumption and without "three wastes" discharging.
Description
The invention belongs to a kind of production and make with extra care 1,2, the novel process of 4-trichlorobenzene.
1,2, the 4-trichlorobenzene is a kind of important chemical material, as sterilant,, also can be used to prepare high boiler, thermal barrier and dielectric liquid etc. as basic material in dyestuff, pharmaceutical industries on agricultural, in all sectors of the national economy purposes is widely arranged.At present, China except that a spot of chemical reagent product is arranged, no large-scale industry products production.By containing 1,2, it is refining 1 more than 99% that the mixed trichlorobenzene crude product of 4-trichlorobenzene 75% prepares purity, 2,4-trichlorobenzene product, the domestic and international method of all using the rectifying of hot method high temperature, but this method facility investment is big, and the raw material consumption height is for example produced a kiloton refining 1 per year, 2, the 4-trichlorobenzene, the rectifying tower cost of stainless steel is about more than 5,000,000 yuan, and raw material consumption height, make with extra care 1,2 for one ton, the 4-trichlorobenzene needs three tons of crude product raw materials.The tail gas of Chan Shenging contains poisonous obnoxious flavour in addition, contains multiple highly toxic substance in the black raffinate.
The objective of the invention is to propose a kind ofly to pay the product mixed trichlorobenzene crude product that invalid body is produced by lindane, it is refining 1,2 to prepare high purity through the cold process crystal refining, the technology of 4-trichlorobenzene.
Main processes of the present invention is: pay the invalid body of product with lindane and carry out alkaline hydrolysis or pyrolysis, make the mixed trichlorobenzene crude product then after separating, dewatering and (wherein contain 1,2,4-trichlorobenzene 75%), when being cooled to 20-30 ℃, crude product under agitation carries out crystallization, stirring velocity 30-40 rev/min, keeping Tc is 5-20 ℃, after the crystallization, with the solid phase liquid phase separation, with activated carbon or potter's clay strainer decolorization filtering, promptly get 1,2,4-trichlorobenzene elaboration, content are more than 99%.If when needing the more highly purified product of preparation, can repeat crystallization 1-2 time.
The cold process crystal refining 1,2 that the present invention proposes, 4-trichlorobenzene novel process, it is few to have a facility investment, and raw material consumption is few, characteristics such as three-waste free discharge.Its investment only is the 10-20% of hot method high temperature rectifying.Raw material consumption also significantly reduces, and the rectifying of hot method high temperature is that 75% thick trichlorobenzene just can prepare one ton of elaboration with three tons of purity, and the cold process crystal refining is that 75% thick trichlorobenzene can be produced one ton of elaboration with two tons of purity only.Adopt processing method of the present invention to produce, no process tail gas, waste liquid, waste water and waste residue, the processing method of genus three-waste free discharge.
Embodiment:
1, lindane is paid the invalid body of product and carried out alkaline hydrolysis or pyrolysis, after separating, dewatering, make the mixed trichlorobenzene crude product then and (wherein contain 1,2,4-trichlorobenzene 75%), when being cooled to 20-30 ℃, crude product under agitation carries out crystallization, stirring velocity 35-40 rev/min, keeping Tc is 5-10 ℃, after the crystallization,, filter with decolorizing with activated carbon with the solid phase liquid phase separation, promptly get 1,2,4-trichlorobenzene elaboration, content are more than 99%.
2, lindane is paid the invalid body of product and carried out alkaline hydrolysis or pyrolysis, after separating, dewatering, make the mixed trichlorobenzene crude product then and (wherein contain 1,2,4-trichlorobenzene 75%), when being cooled to 20-30 ℃, crude product under agitation carries out crystallization, stirring velocity 30-35 rev/min, keeping Tc is 10-15 ℃, after the crystallization, with the solid phase liquid phase separation, with potter's clay strainer decolorization filtering, promptly get 1,2,4-trichlorobenzene elaboration, content are more than 99%.
3, lindane is paid the invalid body of product and carried out alkaline hydrolysis or pyrolysis, after separating, dewatering, make the mixed trichlorobenzene crude product then and (wherein contain 1,2,4-trichlorobenzene 75%), when being cooled to 20-30 ℃, crude product under agitation carries out crystallization, stirring velocity 30-40 rev/min, keeping Tc is 15-20 ℃, after the crystallization, with the solid phase liquid phase separation, with activated carbon or potter's clay strainer decolorization filtering, promptly get 1,2,4-trichlorobenzene elaboration, content are more than 99%.
Claims (1)
1, a kind of production makes with extra care 1,2, the novel process of 4-trichlorobenzene, be to pay invalid body and function alkaline hydrolysis of product or pyrolysis,, under agitation carry out crystallization when it is characterized in that the mixed trichlorobenzene crude product is cooled to 20-30 ℃ through separating, making the mixed trichlorobenzene crude product after the dehydration by lindane, stirring velocity 30-40 rev/min, keeping Tc is 5-20 ℃, after the crystallization, with the solid phase liquid phase separation, with activated carbon or potter's clay strainer decolorization filtering, promptly get 1,2,4-trichlorobenzene elaboration, content are more than 99%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94106841 CN1113907A (en) | 1994-06-22 | 1994-06-22 | Technology for producing refined 2,4-trichloro-benzene |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94106841 CN1113907A (en) | 1994-06-22 | 1994-06-22 | Technology for producing refined 2,4-trichloro-benzene |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1113907A true CN1113907A (en) | 1995-12-27 |
Family
ID=5032681
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94106841 Pending CN1113907A (en) | 1994-06-22 | 1994-06-22 | Technology for producing refined 2,4-trichloro-benzene |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1113907A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225882A (en) * | 2011-05-10 | 2011-10-26 | 浙江永泉化学有限公司 | Method for extracting trichlorobenzene from waste activated carbon |
| CN105859517A (en) * | 2016-05-03 | 2016-08-17 | 四川福思达生物技术开发有限责任公司 | Method for purifying 1,2,4-trichlorobenzene from trichlorobenzene mixture |
| CN105884573A (en) * | 2016-05-06 | 2016-08-24 | 四川福思达生物技术开发有限责任公司 | Preparation method of dicamba |
| CN110128240A (en) * | 2019-06-14 | 2019-08-16 | 河北科技大学 | A kind of method of levitation melting crystallisation separation para chlorobromobenzene and adjacent chloro-bromobenzene |
-
1994
- 1994-06-22 CN CN 94106841 patent/CN1113907A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102225882A (en) * | 2011-05-10 | 2011-10-26 | 浙江永泉化学有限公司 | Method for extracting trichlorobenzene from waste activated carbon |
| CN105859517A (en) * | 2016-05-03 | 2016-08-17 | 四川福思达生物技术开发有限责任公司 | Method for purifying 1,2,4-trichlorobenzene from trichlorobenzene mixture |
| CN105884573A (en) * | 2016-05-06 | 2016-08-24 | 四川福思达生物技术开发有限责任公司 | Preparation method of dicamba |
| CN110128240A (en) * | 2019-06-14 | 2019-08-16 | 河北科技大学 | A kind of method of levitation melting crystallisation separation para chlorobromobenzene and adjacent chloro-bromobenzene |
| CN110128240B (en) * | 2019-06-14 | 2021-11-02 | 河北科技大学 | Method for separating p-chlorobromobenzene and o-chlorobromobenzene by suspension melting crystallization method |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |