CN108238851A - Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols - Google Patents

Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols Download PDF

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Publication number
CN108238851A
CN108238851A CN201711357627.2A CN201711357627A CN108238851A CN 108238851 A CN108238851 A CN 108238851A CN 201711357627 A CN201711357627 A CN 201711357627A CN 108238851 A CN108238851 A CN 108238851A
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CN
China
Prior art keywords
storage tank
alkanisation
centrifuge
antioxidant
butyl
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.)
Withdrawn
Application number
CN201711357627.2A
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Chinese (zh)
Inventor
关艮安
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Chengdu Wijns Technology Co Ltd
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Chengdu Wijns Technology Co Ltd
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Priority to CN201711357627.2A priority Critical patent/CN108238851A/en
Priority to GBGB1722053.4A priority patent/GB201722053D0/en
Publication of CN108238851A publication Critical patent/CN108238851A/en
Priority to AU2018101924A priority patent/AU2018101924A4/en
Withdrawn legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/11—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms
    • C07C37/14—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by reactions increasing the number of carbon atoms by addition reactions, i.e. reactions involving at least one carbon-to-carbon unsaturated bond
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/685—Processes comprising at least two steps in series
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
    • C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
    • C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
    • C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Lubricants (AREA)
  • Anti-Oxidant Or Stabilizer Compositions (AREA)

Abstract

The process units of 2,6 di-t-butyl of antioxidant, 4 methylphenol, mainly includes：Storage tank (F101),Bromobutene gasification tank (F102),Raw material pumps (J101),Alkanisation neutralization reactor (D101),Delivery pump (J102~J105),Alkanisation washing kettle (L101),Centrifuge (L102,L104),Melt washing kettle (L103),Recrystallize reactor (D102),Drying box (L105),Ethanol distillation tower (E101),Condenser (C101),Ethanol storage tank (F103),Wherein,Storage tank (F101) is for storing sulfuric acid,Wherein,Delivery pump (J103) respectively with alkanisation washing kettle (L101),Centrifuge (L102) is connected,Delivery pump (J104) is respectively with recrystallizing reactor (D102),Centrifuge (L104) is connected,Wherein,2.3 2.5m of storage tank (F101) total volume3。

Description

Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols
Technical field
The present invention relates to compound synthesis device more particularly to antioxidant 2, the productions of 6- di-tert-butyl-4-methy phenols Device.
Background technology
2,6- di-tert-butyl-4-methy phenols are a kind of excellent universal phenolic antioxidants, nontoxic, nonflammable, be stale-proof Erosion, excellent storage stability, can inhibit or delay the oxidative degradation of plastics or rubber and prolong the service life.It is various oil products Excellent antioxidant additive, be widely used in various lubricating oil, gasoline, paraffin and various feedstock oils, prevent lubricating oil, fuel oil The rising of acid value or viscosity.It can postpone food as food antioxidant, stabilizer in food grade plastic and packaged food It is rancid.It can be used for polyethylene (PE), polystyrene (PS), PP (polypropylene), polyvinyl chloride, ABS resin, polyester, fiber Plain resin and foamed plastics (especially white or light-colored product), food grade plastic, natural rubber, synthetic rubber (butylbenzene, fourth Nitrile, polyurethane, butadiene rubber etc.), in the products such as animal and plant fat and food, cosmetics containing animal and plant fat.It is existing Process units is mostly more complicated, and 2,6- di-tert-butyl-4-methy phenols are as antioxidant, and process units quality is for improving Product quality, reducing by-products content has Important Economic meaning.
Invention content
The purpose of the present invention is to provide antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols mainly includes： Storage tank (F101), bromobutene gasification tank (F102), raw material pump (J101), alkanisation neutralization reactor (D101), delivery pump (J102~ J105), alkanisation washing kettle (L101), centrifuge (L102, L104), fusing washing kettle (L103), recrystallization reactor (D102), Drying box (L105), ethanol distillation tower (E101), condenser (C101), ethanol storage tank (F103), wherein, storage tank (F101) is used for Sulfuric acid is stored, wherein, delivery pump (J103) is connected respectively with alkanisation washing kettle (L101), centrifuge (L102), delivery pump (J104) it is connected respectively with recrystallization reactor (D102), centrifuge (L104), wherein, storage tank (F101) total volume 2.3- 2.5m3, raw material pump (J101) impeller diameter 130-135mm, recrystallization reactor (D102) outer pot diameter 1200-1250mm.
Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, production procedure are：It will by catalyst of the concentrated sulfuric acid Isobutene reacts 2-3h with paracresol in alkanisation neutralization reaction kettle D101, is neutralized to pH=7 with sodium carbonate after reaction, then 30-50min is washed with water in alkanisation washing kettle L101, ethyl alcohol coarse crystallization is used after separating water layer.After centrifuge L102 filterings, Fusing in washing kettle L103, washing are melted, separates water layer.Ethyl alcohol recrystallization is used again in reactor D102 is recrystallized.Through L104 It centrifuges, L105 is drying to obtain finished product.The invention has the advantages that：Reduce reaction intermediate link, reduce reaction temperature and Reaction time improves reaction yield.
Description of the drawings
Fig. 1 is antioxidant 2, and the process units of 6- di-tert-butyl-4-methy phenols mainly includes：Storage tank (F101), bromine fourth Alkene gasification tank (F102), raw material pump (J101), alkanisation neutralization reactor (D101), delivery pump (J102~J105), alkanisation washing Kettle (L101), centrifuge (L102, L104), fusing washing kettle (L103), recrystallization reactor (D102), drying box (L105), Ethanol distillation tower (E101), condenser (C101), ethanol storage tank (F103).
Specific embodiment
With reference to specific implementation example, the invention will be further described：
Example 1：
Raw materials for production and dosage
P-cresol Technical grade, >=98% 1500kg
Isobutene Technical grade, >=90% 2400kg
Ethyl alcohol Technical grade, 95% 1000kg
The concentrated sulfuric acid Technical grade, 98% 70kg
Sodium carbonate Technical grade In right amount
Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, mainly includes：Storage tank (F101), bromobutene gas Change tank (F102), raw material pump (J101), alkanisation neutralization reactor (D101), delivery pump (J102~J105), alkanisation washing kettle (L101), centrifuge (L102, L104), fusing washing kettle (L103), recrystallization reactor (D102), drying box (L105), second Alcohol destilling tower (E101), condenser (C101), ethanol storage tank (F103), wherein, storage tank (F101) for storing sulfuric acid, wherein, Delivery pump (J103) is connected respectively with alkanisation washing kettle (L101), centrifuge (L102), and delivery pump (J104) is respectively with tying again Brilliant reactor (D102), centrifuge (L104) are connected, wherein, storage tank (F101) total volume 2.3m3, raw material pump (J101) impeller Diameter 130mm, recrystallization reactor (D102) outer pot diameter 1200mm.
Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, production procedure are：It will by catalyst of the concentrated sulfuric acid Isobutene reacts 2h with paracresol in alkanisation neutralization reaction kettle D101, is neutralized to pH=7 with sodium carbonate after reaction, then 30min is washed with water in alkanisation washing kettle L101, ethyl alcohol coarse crystallization is used after separating water layer.After centrifuge L102 filterings, melting Fusing, washing, separate water layer in washing kettle L103.Ethyl alcohol recrystallization is used again in reactor D102 is recrystallized.It is centrifuged through L104 Separation, L105 are drying to obtain finished product.
Final product quality
Example 2：
Raw materials for production and dosage
Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, mainly includes：Storage tank (F101), bromobutene gas Change tank (F102), raw material pump (J101), alkanisation neutralization reactor (D101), delivery pump (J102~J105), alkanisation washing kettle (L101), centrifuge (L102, L104), fusing washing kettle (L103), recrystallization reactor (D102), drying box (L105), second Alcohol destilling tower (E101), condenser (C101), ethanol storage tank (F103), wherein, storage tank (F101) for storing sulfuric acid, wherein, Delivery pump (J103) is connected respectively with alkanisation washing kettle (L101), centrifuge (L102), and delivery pump (J104) is respectively with tying again Brilliant reactor (D102), centrifuge (L104) are connected, wherein, storage tank (F101) total volume 2.5m3, raw material pump (J101) impeller Diameter 135mm, recrystallization reactor (D102) outer pot diameter 1250mm.
Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, production procedure are：It will by catalyst of the concentrated sulfuric acid Isobutene reacts 3h with paracresol in alkanisation neutralization reaction kettle D101, is neutralized to pH=7 with sodium carbonate after reaction, then 50min is washed with water in alkanisation washing kettle L101, ethyl alcohol coarse crystallization is used after separating water layer.After centrifuge L102 filterings, melting Fusing, washing, separate water layer in washing kettle L103.Ethyl alcohol recrystallization is used again in reactor D102 is recrystallized.It is centrifuged through L104 Separation, L105 are drying to obtain finished product.
Final product quality
It described in above example, is merely preferred embodiments of the present invention, but protection scope of the present invention not office Be limited to this, any one skilled in the art in the technical scope disclosed by the present invention, the technique according to the invention Scheme and its inventive concept are subject to equivalent substitution or change, should be covered by the protection scope of the present invention.

Claims (3)

1. antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols, which is characterized in that mainly include：Storage tank (F101), Bromobutene gasification tank (F102), raw material pump (J101), alkanisation neutralization reactor (D101), delivery pump (J102~J105), alkanisation Washing kettle (L101), centrifuge (L102, L104), fusing washing kettle (L103), recrystallization reactor (D102), drying box (L105), ethanol distillation tower (E101), condenser (C101), ethanol storage tank (F103), wherein, storage tank (F101) is for storing sulphur Acid, wherein, delivery pump (J103) is connected respectively with alkanisation washing kettle (L101), centrifuge (L102), delivery pump (J104) point It is not connected with recrystallization reactor (D102), centrifuge (L104), wherein, storage tank (F101) total volume 2.3-2.5m3。
2. antioxidant 2 according to claim 1, the process units of 6- di-tert-butyl-4-methy phenols, which is characterized in that institute Raw material pump (J101) the impeller diameter 130-135mm stated.
3. antioxidant 2 according to claim 1, the process units of 6- di-tert-butyl-4-methy phenols, which is characterized in that institute Recrystallization reactor (D102) the outer pot diameter 1200-1250mm stated.
CN201711357627.2A 2017-12-16 2017-12-16 Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols Withdrawn CN108238851A (en)

Priority Applications (3)

Application Number Priority Date Filing Date Title
CN201711357627.2A CN108238851A (en) 2017-12-16 2017-12-16 Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols
GBGB1722053.4A GB201722053D0 (en) 2017-12-16 2017-12-28 Antioxidant 2,6-di-tert-butyl-4-methylphenol production plant
AU2018101924A AU2018101924A4 (en) 2017-12-16 2018-12-03 Antioxidant 2,6-di-tert-butyl-4-methylphenol production plant

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Application Number Priority Date Filing Date Title
CN201711357627.2A CN108238851A (en) 2017-12-16 2017-12-16 Antioxidant 2, the process units of 6- di-tert-butyl-4-methy phenols

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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AU2018101924A4 (en) 2019-01-31

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