CN105541560A - TBHQ crude product synthesis process - Google Patents
TBHQ crude product synthesis process Download PDFInfo
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- CN105541560A CN105541560A CN201410583769.0A CN201410583769A CN105541560A CN 105541560 A CN105541560 A CN 105541560A CN 201410583769 A CN201410583769 A CN 201410583769A CN 105541560 A CN105541560 A CN 105541560A
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- crude product
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- tbhq crude
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Abstract
The present invention discloses a TBHQ crude product synthesis process, which comprises: 1) pouring 2-5 parts by weight of phosphoric acid and 0.2-0.5 part by weight of water into a stirring jar, adding 4-6 parts by weight of hydroquinone to the stirring jar, and stirring; 2) after the stirring, placing the mixed solution into a reaction kettle, heating to a temperature of 50-69 DEG C, and pouring 7-10 parts by weight of tert-butanol to the reaction kettle; 3) heating to a temperature of 73-83 DEG C, carrying out thermal insulation for 2-3 h, and carrying out a reaction; and 4) carrying out centrifugation separation on the reaction product, carrying out water washing, and dewatering to obtain the TBHQ crude product. According to the TBHQ crude product preparation process of the present invention, the water is adopted as the solvent while the use of the toluene as the solvent is abandoned, such that the pollution is low, the raw material utilization rate is high, and the TBHQ purity in the obtained TBHQ crude product is high.
Description
Technical field
The invention belongs to chemical technique field, be specifically related to a kind of synthesis technique of TBHQ crude product.
Background technology
The synthesis technique of TBHQ crude product at least comprises the primary processes such as centrifugation, washing, dehydration.In the synthesis technique of current TBHQ crude product, technical process is not easy to implement, and separation efficiency is low, can not achieve recycling of raw material, and production process is complicated, and production efficiency is low.
Summary of the invention
In order to overcome the above-mentioned technical problem that prior art field exists, the object of the invention is to, a kind of synthesis technique of TBHQ crude product is provided, the present invention not only production process simple, increase work efficiency, and achieve the guarantee of quality product.
The synthesis technique of TBHQ crude product provided by the invention, comprises the following steps:
(1) water of the phosphoric acid of 2 – 5 weight parts, 0.2 – 0.5 weight part is poured in a mixing bowl, then stir to the Resorcinol that a mixing bowl adds 4 – 6 weight parts;
(2) after stirring, mixing solutions is inserted in reactor and be heated to 50 DEG C ~ 69 DEG C, then add the trimethyl carbinol of 7 – 10 weight parts to reactor;
(3), after continuing to be heated to 73 DEG C ~ 83 DEG C, be incubated and react for 2 ~ 3 hours;
(4) namely reaction product is obtained TBHQ crude product after centrifugation, washing, dehydration.
The synthesis technique of TBHQ crude product provided by the invention, its beneficial effect is, overcoming prior art, to prepare operation in TBHQ crude product process more, and the problem that workload is large, improves working efficiency; Improve the utilization ratio of reactant and the yield of product.
Embodiment
Below in conjunction with an embodiment, the synthesis technique of TBHQ crude product provided by the invention is described in detail.
Embodiment
The synthesis technique of the TBHQ crude product of the present embodiment, comprises the following steps:
(1) water of the phosphoric acid of 5 weight parts, 0.5 weight part is poured in a mixing bowl, then stir to the Resorcinol that a mixing bowl adds 4 weight parts;
(2) after stirring, mixing solutions is inserted in reactor and be heated to 69 DEG C, then add the trimethyl carbinol of 10 weight parts to reactor;
(3), after continuing to be heated to 83 DEG C, be incubated and react for 3 hours;
(4) namely reaction product is obtained TBHQ crude product after centrifugation, washing, dehydration.
The synthesis technique of TBHQ crude product, can directly prepare TBHQ crude product, and without the need to further processing, operation is simple, and take off data is accurate, easy to implement.
Claims (1)
1. a synthesis technique for TBHQ crude product, is characterized in that: said method comprising the steps of:
(1) water of the phosphoric acid of 2 – 5 weight parts, 0.2 – 0.5 weight part is poured in a mixing bowl, then stir to the Resorcinol that a mixing bowl adds 4 – 6 weight parts;
(2) after stirring, mixing solutions is inserted in reactor and be heated to 50 DEG C ~ 69 DEG C, then add the trimethyl carbinol of 7 – 10 weight parts to reactor;
(3), after continuing to be heated to 73 DEG C ~ 83 DEG C, be incubated and react for 2 ~ 3 hours;
(4) namely reaction product is obtained TBHQ crude product after centrifugation, washing, dehydration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410583769.0A CN105541560A (en) | 2014-10-28 | 2014-10-28 | TBHQ crude product synthesis process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410583769.0A CN105541560A (en) | 2014-10-28 | 2014-10-28 | TBHQ crude product synthesis process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105541560A true CN105541560A (en) | 2016-05-04 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201410583769.0A Pending CN105541560A (en) | 2014-10-28 | 2014-10-28 | TBHQ crude product synthesis process |
Country Status (1)
| Country | Link |
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| CN (1) | CN105541560A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878008A (en) * | 2018-09-06 | 2020-03-13 | 天津科伦药物研究有限公司 | Preparation method of high-purity 2-tert-butylhydroquinone and purification method of 2-tert-butylhydroquinone |
| CN112479828A (en) * | 2020-12-17 | 2021-03-12 | 厦门大学 | Synthetic method of tert-butyl hydroquinone |
-
2014
- 2014-10-28 CN CN201410583769.0A patent/CN105541560A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878008A (en) * | 2018-09-06 | 2020-03-13 | 天津科伦药物研究有限公司 | Preparation method of high-purity 2-tert-butylhydroquinone and purification method of 2-tert-butylhydroquinone |
| CN110878008B (en) * | 2018-09-06 | 2023-10-13 | 四川科伦药物研究院有限公司 | Preparation method of high-purity 2-tertiary butyl hydroquinone and purification method of 2-tertiary butyl hydroquinone |
| CN112479828A (en) * | 2020-12-17 | 2021-03-12 | 厦门大学 | Synthetic method of tert-butyl hydroquinone |
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Legal Events
| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20160504 |