CN1313270A - Process for preparing 2,6-di-tear-butyl p-cresol - Google Patents
Process for preparing 2,6-di-tear-butyl p-cresol Download PDFInfo
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- CN1313270A CN1313270A CN 00110191 CN00110191A CN1313270A CN 1313270 A CN1313270 A CN 1313270A CN 00110191 CN00110191 CN 00110191 CN 00110191 A CN00110191 A CN 00110191A CN 1313270 A CN1313270 A CN 1313270A
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Abstract
A process for preparing 2,6-di-tert-butyl p-cresol from isobutylene features that the processed ion exchange resin is used as catalyst, the ratio of p-cresol to catalyst is 1:(0.1-0.4) and two reactors are serially communicated, and includes such steps as adding isometric catalyst and p-cresol to both reactors, ordinary-pressure stirring while introducing gasified isobutylene, reacting at 50-130 deg.C, refining in rectification tower, recrystallizing and drying. Its advantages include no generation of waste water, low cost, and high quality of finished product.
Description
The present invention relates to C07C 39/06 alkylated benzenes phenols, a kind of novel process for preparing 2,6 ditertiary butyl p cresol.
2,6 ditertiary butyl p cresol (BHT) is commonly called as antioxidant 264, and petroleum refining industry claims T501, is the especially irreplaceable good oxidation inhibitor of lubricating oil of various oil products, is the not tint permanence oxidation inhibitor of a kind of multi-usage, world's consumption maximum.
Produce at present both at home and abroad the technology of this antioxidant BHT, mostly adopt iso-butylene to make alkylating agent, with the vitriol oil, aromatic sulfonic acid or solid acid as catalyst and p-cresol at normal pressure or add and depress prepared in reaction.Alkylation liquid by method for preparing neutralizes through yellow soda ash, washes 2-3 time, and water consumption is approximately 1 times of reactant volume, to remove catalyzer.Produce a large amount of phenolic wastewater in the water washing process, need just can reach national specified discharge standard through removing the phenol processing, and serious with this type of catalyzer to equipment corrosion.Essential corrosion resistant apparatus and the waste water disposal facility of adopting must increase facility investment, and cost is improved.The waste water of domestic most of producers after simple process, dilution discharge, the cumulative total amount of pollutant still pollutes environment.
The purpose of this invention is to provide a kind of novel process for preparing 2,6 ditertiary butyl p cresol, adopt resin to make catalyzer, do not wash with water, do not produce phenolic wastewater, equipment is not had corrosion.
The novel process of preparation 2,6 ditertiary butyl p cresol of the present invention adopts pure iso-butylene to make raw material, makes catalyzer with the ion exchange resin of treated mistake, reacts through two placed in-line reactors and p-cresol under normal pressure; The catalyzer and the p-cresol that in two stills, add equivalent respectively, make still be warmed up to 50 ℃ then, iso-butylene after under normal pressure stirs, in still 1, feeding gasification, temperature of reaction is controlled at 50-130 ℃, the inlet amount of control iso-butylene, the composition of stratographic analysis alkylation liquid is made in sampling, p-cresol is reacted completely reach reaction end; It is refining that alkylation liquid is sent to rectifying tower, and the BHT after the rectifying gets finished product again after recrystallization, drying.
The ion-exchange resin catalyst of this process using must be handled through chemistry, physical method, and reusable, be several thousand hours its work-ing life, when this activity of such catalysts is reduced to a half, treated just renewable in former still.This catalyzer does not wash the alkylation liquid of this technology with water, directly sends to refining.Product separates easily with catalyzer, and catalyzer does not have corrosion to equipment, does not produce waste water, saves the bulky equipment investment of sewage disposal, and is especially significant to the protection environment.The characteristics of this technology be cost low, not without dye, the final product quality height, BHT can reach the state food level, meets the GB1900-80 standard.
Embodiment:
Preparation 2, the novel process of 6-ditertbutylparacresol, the pure iso-butylene raw material that adopts is from methyl tertiary butyl ether (MTBE) cracker, purity 〉=99%, the purity of p-cresol 〉=98%, it is characterized in that catalyzer adopts the ion exchange resin of handling through chemistry, physical method, two reactor series connection; Still 1 is emitted tail gas, absorbs through still 2, guarantees that isobutene reaction is complete.The catalyzer and the p-cresol that add equivalent in two stills respectively, p-cresol and catalyzer be by weight: 1: 0.1-0.4; Make still be warmed up to 50 ℃ then, iso-butylene after under normal pressure stirs, in still 1, feeding gasification, temperature of reaction is controlled at 50-130 ℃, the inlet amount of control iso-butylene, the mol ratio of p-cresol and iso-butylene is 1: 2, the composition of stratographic analysis alkylation liquid is made in sampling, and p-cresol is reacted completely, and reaches reaction end; After reaction is finished alkylation liquid is sent to rectifying tower and make with extra care, catalyzer is stayed in the still and is reused; BHT after the rectifying gets finished product again after recrystallization, drying.Finished product is a white crystals, fusing point: 69-70 ℃, meets state food level GB1900-80 standard.
Claims (2)
1, a kind of novel process for preparing 2,6 ditertiary butyl p cresol adopts pure iso-butylene to make raw material, makes catalyzer with the ion exchange resin of handling, and reacts through two placed in-line reactors and p-cresol under normal pressure; The catalyzer and the p-cresol that in two stills, add equivalent respectively, make still be warmed up to 50 ℃ then, iso-butylene after under normal pressure stirs, in still 1, feeding gasification, temperature of reaction is controlled at 50-130 ℃, the inlet amount of control iso-butylene, the composition of sampling analysis alkylation liquid, still 1 is emitted tail gas, absorb through still 2, p-cresol is reacted completely reach reaction end; It is refining that alkylation liquid is sent into rectifying tower, and catalyzer is stayed in the still and reused; BHT after the rectifying again through recrystallization, again after recrystallization, drying finished product.
2, technology according to claim 1 is characterized in that p-cresol and catalyzer are by weight 1: 0.1-0.4; The mol ratio of p-cresol and iso-butylene is 1: 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110191 CN1313270A (en) | 2000-03-13 | 2000-03-13 | Process for preparing 2,6-di-tear-butyl p-cresol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 00110191 CN1313270A (en) | 2000-03-13 | 2000-03-13 | Process for preparing 2,6-di-tear-butyl p-cresol |
Publications (1)
| Publication Number | Publication Date |
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| CN1313270A true CN1313270A (en) | 2001-09-19 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 00110191 Pending CN1313270A (en) | 2000-03-13 | 2000-03-13 | Process for preparing 2,6-di-tear-butyl p-cresol |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410224C (en) * | 2006-11-07 | 2008-08-13 | 中唯炼焦技术国家工程研究中心有限责任公司 | New method of preparing tert-butyl phenol by alkylation of phenol and isobutene |
| CN100447121C (en) * | 2006-07-15 | 2008-12-31 | 孟祥儒 | Production process of antioxidant 2,6-di-tert-butyl-4-methy phenol |
| CN103694085A (en) * | 2013-12-31 | 2014-04-02 | 江苏迈达投资发展股份有限公司 | Crystallization method of high-purity antioxidant BHT (butylated hydroxytoluene) |
| CN104496758A (en) * | 2014-12-02 | 2015-04-08 | 安徽海华科技股份有限公司 | M-cresol and p-cresol alkylated continuous reaction method |
| CN106866380A (en) * | 2017-02-20 | 2017-06-20 | 河北工业大学 | A kind of micro- reactive distillation plate prepares the method and its equipment of 2,6 BHTs |
| CN107649170A (en) * | 2017-09-30 | 2018-02-02 | 宝鸡文理学院 | A kind of carried molecular sieve catalyst for synthesizing the DI-tert-butylphenol compounds of 4 methyl 2,6 and its application |
| CN111233634A (en) * | 2020-02-29 | 2020-06-05 | 陕西宝塔山新材料有限公司 | Method for controlling antioxidant BHT crystallization by program forced cooling |
| CN111943816A (en) * | 2020-07-23 | 2020-11-17 | 安徽海华科技有限公司 | Preparation method of high-purity 2, 6-di-tert-butyl-p-cresol |
| CN112694389A (en) * | 2020-12-25 | 2021-04-23 | 南京晶典抗氧化技术研究院有限公司 | Synthesis method for synthesizing 2,6 di-tert-butyltoluene through heterogeneous catalysis |
| CN113248349A (en) * | 2021-06-16 | 2021-08-13 | 南京元素科技有限公司 | Device for alkylation continuous reaction of m-cresol and/or p-cresol |
| CN113880696A (en) * | 2021-10-09 | 2022-01-04 | 陕西万汇能聚科技有限公司 | Separation and purification method of m-cresol and p-cresol |
-
2000
- 2000-03-13 CN CN 00110191 patent/CN1313270A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100447121C (en) * | 2006-07-15 | 2008-12-31 | 孟祥儒 | Production process of antioxidant 2,6-di-tert-butyl-4-methy phenol |
| CN100410224C (en) * | 2006-11-07 | 2008-08-13 | 中唯炼焦技术国家工程研究中心有限责任公司 | New method of preparing tert-butyl phenol by alkylation of phenol and isobutene |
| CN103694085A (en) * | 2013-12-31 | 2014-04-02 | 江苏迈达投资发展股份有限公司 | Crystallization method of high-purity antioxidant BHT (butylated hydroxytoluene) |
| CN103694085B (en) * | 2013-12-31 | 2016-08-17 | 江苏迈达投资发展股份有限公司 | A kind of highly purified antioxidant BHT method for crystallising |
| CN104496758A (en) * | 2014-12-02 | 2015-04-08 | 安徽海华科技股份有限公司 | M-cresol and p-cresol alkylated continuous reaction method |
| CN106866380B (en) * | 2017-02-20 | 2020-04-07 | 河北工业大学 | Method and equipment for preparing 2, 6-di-tert-butyl-p-cresol by using micro-reaction rectifying plate |
| CN106866380A (en) * | 2017-02-20 | 2017-06-20 | 河北工业大学 | A kind of micro- reactive distillation plate prepares the method and its equipment of 2,6 BHTs |
| CN107649170A (en) * | 2017-09-30 | 2018-02-02 | 宝鸡文理学院 | A kind of carried molecular sieve catalyst for synthesizing the DI-tert-butylphenol compounds of 4 methyl 2,6 and its application |
| CN107649170B (en) * | 2017-09-30 | 2020-02-21 | 宝鸡文理学院 | Supported molecular sieve catalyst for synthesizing 4-methyl-2, 6-di-tert-butylphenol and application thereof |
| CN111233634A (en) * | 2020-02-29 | 2020-06-05 | 陕西宝塔山新材料有限公司 | Method for controlling antioxidant BHT crystallization by program forced cooling |
| CN111233634B (en) * | 2020-02-29 | 2022-10-18 | 陕西宝塔山新材料有限公司 | Method for controlling antioxidant BHT crystallization by program forced cooling |
| CN111943816A (en) * | 2020-07-23 | 2020-11-17 | 安徽海华科技有限公司 | Preparation method of high-purity 2, 6-di-tert-butyl-p-cresol |
| CN112694389A (en) * | 2020-12-25 | 2021-04-23 | 南京晶典抗氧化技术研究院有限公司 | Synthesis method for synthesizing 2,6 di-tert-butyltoluene through heterogeneous catalysis |
| CN113248349A (en) * | 2021-06-16 | 2021-08-13 | 南京元素科技有限公司 | Device for alkylation continuous reaction of m-cresol and/or p-cresol |
| CN113880696A (en) * | 2021-10-09 | 2022-01-04 | 陕西万汇能聚科技有限公司 | Separation and purification method of m-cresol and p-cresol |
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