AU2018101932A4 - 2-hydroxy-4-octoxybenzophenone production plant - Google Patents

2-hydroxy-4-octoxybenzophenone production plant Download PDF

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AU2018101932A4
AU2018101932A4 AU2018101932A AU2018101932A AU2018101932A4 AU 2018101932 A4 AU2018101932 A4 AU 2018101932A4 AU 2018101932 A AU2018101932 A AU 2018101932A AU 2018101932 A AU2018101932 A AU 2018101932A AU 2018101932 A4 AU2018101932 A4 AU 2018101932A4
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tank
reactor
chlorination
store
distillation column
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AU2018101932A
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genan guan
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Chengdu Wei En Si Technology Co Ltd
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Chengdu Wei En Si Technology Co Ltd
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C17/00—Preparation of halogenated hydrocarbons
    • C07C17/093—Preparation of halogenated hydrocarbons by replacement by halogens
    • C07C17/10—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms
    • C07C17/12—Preparation of halogenated hydrocarbons by replacement by halogens of hydrogen atoms in the ring of aromatic compounds
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/42—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis
    • C07C45/43—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by hydrolysis of >CX2 groups, X being halogen
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
    • C07C45/61—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups
    • C07C45/64—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds by reactions not involving the formation of >C = O groups by introduction of functional groups containing oxygen only in singly bound form

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Low-Molecular Organic Synthesis Reactions Using Catalysts (AREA)

Abstract

2-hydroxy-4-octoxybenzophenone production plant Abstract 5 2-hydroxy-4-octoxybenzophenone production plant, including: tank (F101), chlorination reactor (DI01), transfer pump (J1O-J107), synthesis reactor (D102), centrifuge (LIO, L104, L105), drying oven (L102), condenser (C101-C104), finished product synthetic reactor (D104), recrystallization reactor (DI05), chlorination kettle (D103), chlorination water washing tank (D104), drying kettle 10 (L103), distillation column (ElOl), tank (F102), tank (F103), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column (E103), tank (F105); among them, tank (FlOl) is used to store liquid chlorine, tank (F102) is used to store previous fraction, tank (F103) is used to store chlorinated n-octane, tank (F104) is used to store cyclohexanone, tank (F104) is used to store ethanol; among 15 them, transfer pump (JIO) is connected respectively to chlorination reactor (DI01) and synthesis reactor (D102), transfer pump (J103) is connected respectively to drying oven (L102) and finished product synthetic reactor (D104); among them, cylinder diameter of tank (F101) is 900-1000 mm. 20 Figure 1 -- Fiu 1 - Figure 1

Description

2-hydroxy-4-octoxybenzophenone production plant
2018101932 03 Dec 2018
FIELD OF THE INVENTION
The present invention relates to a kind of pharmaceutical synthesis plant, more particularly, relates to 2-hydroxy-4-octoxybenzophenone production plant
GENERAL BACKGROUND
2-hydroxy-4-octoxybenzophenone can strongly absorb UV rays of 300-375 nm and is compatible with most polymers, especially with polyolefins. It is almost colorless, with low volatility. This product is mainly suitable for polyolefins, and also for plastics, fibers and coatings of vinyl, polystyrene, cellulose plastics, polyesters, polyamides, and so on. The dosage in plastic: polyolefin 0.25-1.0 parts; hard PVC 0.25-0.5 parts; polypropylene fiber and acrylic about 0.5 parts. Most of the existing production plant processes are complex. Thus, as a UV absorber, the advantages and disadvantages of production equipment of 2-hydroxy-4-octoxybenzophenone have a great economic significant for improving product quality and reducing the by-product contents.
SUMMARY
The purpose of the present invention is to provide 2-hydroxy-4-octoxybenzophenone production plant, including: tank (Fl 01), chlorination reactor (D101), transfer pump (J101-J107), synthesis reactor (D102), centrifuge (L101, LI04, LI05), drying oven (LI02), condenser (C101-C104), finished product synthetic reactor (DI 04), recrystallization reactor (DI 05), chlorination kettle (DI03), chlorination water washing tank (DI04), drying kettle (L103), distillation column (E101), tank (F102), tank (F103), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column (E103), tank (Fl05); among them, tank (Fl01) is used to store liquid chlorine, tank (Fl02) is used to store previous fraction, tank (Fl03) is used to store chlorinated n-octane, tank (F104) is used to store cyclohexanone, tank (F104) is used to store ethanol; among them, transfer pump (JI01) is connected respectively to chlorination reactor (DI01)
2018101932 03 Dec 2018 and synthesis reactor (DI02), transfer pump (JI03) is connected respectively to drying oven (LI02) and finished product synthetic reactor (DI04); among them, cylinder diameter of tank (F101) is 900-1000 mm, nominal volume of chlorination reactor (D101) is 800-900 L, heat pipe diameter of condenser (C101) is 0.013-0.014 m.
2-hydroxy-4-octoxybenzophenone production plant, the production process is:
chlorinated toluene with chlorine in chlorination reactor D101 to generate trichlorotoluene, which is used to react with resorcinol solution in ethanol in synthesis reactor DI02. The reaction temperature is 30-36 °C, the time is 2-3 h, that generates 2,4-dihydroxybenzophenone. Filtered, washed, and dried for standby application. In 10 chlorination kettle DI03, used zinc chloride as a dehydration catalyst, n-octanol reacts with concentrated hydrochloric acid to generate 1-chloro-n-octane crude product. Washed in chlorinated water washing tank DI04, dried with anhydrous calcium chloride in drying tank LI03, distilled to obtain fine 1-chloro-n-octane in distillation tank E101. In finished product synthetic reactor DI04, used soda ash and potassium 15 iodide as catalyst, reacted with dried 2,4-dihydroxybenzophenone in a solvent cyclohexanone, stirred, refluxed and filtered to obtain the crude product, rectified by ethanol in recrystallization reactor (DI05), filtered and obtained the finished product. Among them, waste cyclohexanone and waste ethanol are respectively recycled after distillation in cyclohexanone distillation column El02 and ethanol distillation column 20 El03. The advantages of this invention are that the reaction time is reduced and the reaction rate is improved.
DESCRIPTION OF THE DRAWINGS
Figure 1 is 2-hydroxy-4-octoxybenzophenone production plant.
Include: tank (F101), chlorination reactor (D101), transfer pump (J101-J107), synthesis reactor (DI02), centrifuge (LI01, LI04, LI05), drying oven (LI02), condenser (C101-C104), finished product synthetic reactor (DI04), recrystallization reactor (DI05), chlorination kettle (DI03), chlorination water washing tank (DI04), drying kettle (LI03), distillation column (El01), tank (Fl02), tank (Fl03), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column 30 (El03), tank (Fl05);
2018101932 03 Dec 2018
DETAILED DESCRIPTION OF PREFERRED EMBODIMENTS
The following examples with reference to specific embodiments of the present invention are further illustrated:
Embodiment 1
Raw materials and dosages
Toluene Industrial grade 900 kg Zinc chloride Industrial grade Appropriate amount
Resorcinol Industrial grade, >95% 1100 kg Concentrated hydrochloric acid Industrial grade, 35% Appropriate amount
N-octanol Industrial grade 1300 kg Anhydrous calcium chloride Industrial grade Appropriate amount
Chlorine Industrial grade, >95% 2000 kg Soda ash Industrial grade Appropriate amount
Cyclohexanone Industrial grade 1200 kg Potassium iodide Industrial grade Appropriate amount
Ethanol Industrial grade, 95% Appropriate amount
2-hydroxy-4-octoxybenzophenone production plant, including: tank (Fl01), chlorination reactor (D101), transfer pump (J101-J107), synthesis reactor (D102), centrifuge (L101, LI04, LI05), drying oven (LI02), condenser (C101-C104), finished product synthetic reactor (DI 04), recrystallization reactor (DI 05), chlorination kettle (DI03), chlorination water washing tank (DI04), drying kettle (L103), distillation column (E101), tank (F102), tank (F103), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column (E103), tank (Fl05); among them, tank (Fl01) is used to store liquid chlorine, tank (Fl02) is used to store previous fraction, tank (Fl03) is used to store chlorinated n-octane, tank (F104) is used to store cyclohexanone, tank (F104) is used to store ethanol; among them, transfer pump (JI01) is connected respectively to chlorination reactor (DI01)
2018101932 03 Dec 2018 and synthesis reactor (DI02), transfer pump (JI03) is connected respectively to drying oven (LI02) and finished product synthetic reactor (DI04); among them, cylinder diameter of tank (Fl 01) is 900 mm, nominal volume of chlorination reactor (D101) is
800 L, heat pipe diameter of condenser (C101) is 0.013 m.
2-hydroxy-4-octoxybenzophenone production plant, the production process is:
chlorinated toluene with chlorine in chlorination reactor D101 to generate trichlorotoluene, which is used to react with resorcinol solution in ethanol in synthesis reactor DI02. The reaction temperature is 30 °C, the time is 2 h, that generates 2,4-dihydroxybenzophenone. Filtered, washed, and dried for standby application. In 10 chlorination kettle DI03, used zinc chloride as a dehydration catalyst, n-octanol reacts with concentrated hydrochloric acid to generate 1-chloro-n-octane crude product. Washed in chlorinated water washing tank DI04, dried with anhydrous calcium chloride in drying tank LI03, distilled to obtain fine 1-chloro-n-octane in distillation tank E101. In finished product synthetic reactor DI04, used soda ash and potassium 15 iodide as catalyst, reacted with dried 2,4-dihydroxybenzophenone in a solvent cyclohexanone, stirred, refluxed and filtered to obtain the crude product, rectified by ethanol in recrystallization reactor (DI05), filtered and obtained the finished product. Among them, waste cyclohexanone and waste ethanol are respectively recycled after distillation in cyclohexanone distillation column El02 and ethanol distillation column 20 E103.
The qualities of the product are as follows:
Exterior Light yellow or white crystalline powder
Density (25 °C) 1.162 g/cm3
Melting point 46 °C
Solubility (g/lOOg, 25°C) Benzene 72.2, 95% ethanol 2.6, hexane 40.1, acetone 74.3, slightly soluble in dichloroethane
Embodiment 2
Raw materials and dosages
2018101932 03 Dec 2018
Toluene Industrial grade 1000 kg Zinc chloride Industrial grade Appropriate amount
Resorcinol Industrial grade, >95% 1200 kg Concentrated hydrochloric acid Industrial grade, 35% Appropriate amount
N-octanol Industrial grade 1300 kg Anhydrous calcium chloride Industrial grade Appropriate amount
Chlorine Industrial grade, >95% 2100 kg Soda ash Industrial grade Appropriate amount
Cyclohexanone Industrial grade 1300 kg Potassium iodide Industrial grade Appropriate amount
Ethanol Industrial grade, 95% Appropriate amount
2-hydroxy-4-octoxybenzophenone production plant, including: tank (F101), chlorination reactor (D101), transfer pump (J101-J107), synthesis reactor (D102), centrifuge (L101, LI04, LI05), drying oven (LI02), condenser (C101-C104), finished product synthetic reactor (DI 04), recrystallization reactor (DI 05), 5 chlorination kettle (DI03), chlorination water washing tank (DI04), drying kettle (L103), distillation column (E101), tank (F102), tank (F103), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column (E103), tank (Fl05); among them, tank (Fl01) is used to store liquid chlorine, tank (Fl02) is used to store previous fraction, tank (Fl03) is used to store chlorinated n-octane, tank 10 (F104) is used to store cyclohexanone, tank (F104) is used to store ethanol; among them, transfer pump (JI01) is connected respectively to chlorination reactor (DI01) and synthesis reactor (DI02), transfer pump (JI03) is connected respectively to drying oven (LI02) and finished product synthetic reactor (DI04); among them, cylinder diameter of tank (F101) is 1000 mm, nominal volume of chlorination reactor (D101) 15 is 900 L, heat pipe diameter of condenser (C101) is 0.014 m.
2-hydroxy-4-octoxybenzophenone production plant, the production process is: chlorinated toluene with chlorine in chlorination reactor D101 to generate
2018101932 03 Dec 2018 trichlorotoluene, which is used to react with resorcinol solution in ethanol in synthesis reactor DI02. The reaction temperature is 36 °C, the time is 3 h, that generates
2,4-dihydroxybenzophenone. Filtered, washed, and dried for standby application. In chlorination kettle D103, used zinc chloride as a dehydration catalyst, n-octanol reacts with concentrated hydrochloric acid to generate 1-chloro-n-octane crude product.
Washed in chlorinated water washing tank DI04, dried with anhydrous calcium chloride in drying tank LI03, distilled to obtain fine 1-chloro-n-octane in distillation tank E101. In finished product synthetic reactor DI04, used soda ash and potassium iodide as catalyst, reacted with dried 2,4-dihydroxybenzophenone in a solvent 10 cyclohexanone, stirred, refluxed and filtered to obtain the crude product, rectified by ethanol in recrystallization reactor (DI05), filtered and obtained the finished product.
Among them, waste cyclohexanone and waste ethanol are respectively recycled after distillation in cyclohexanone distillation column El02 and ethanol distillation column E103.
The qualities of the product are as follows:
Exterior Light yellow or white crystalline powder
Density (25 °C) 1.165 g/cm3
Melting point 47 °C
Solubility (g/lOOg, 25 °C) Benzene 72.2, 95% ethanol 2.6, hexane 40.1, acetone 74.3, slightly soluble in dichloroethane
The embodiments of the present invention are merely preferred embodiments of the present invention, but the range of the present invention is not limited this, and any person who is familiar with those skilled in the arts, within the technical range of the present invention. It is intended that the technical solution and its inventive 20 concept be replaced or modified equivalently with reference to the range of the invention.

Claims (3)

1. 2-hydroxy-4-octoxybenzophenone production plant, including: tank (F101), chlorination reactor (D101), transfer pump (J101-J107), synthesis reactor (D102),
5 centrifuge (L101, LI04, LI05), drying oven (LI02), condenser (C101-C104), finished product synthetic reactor (DI 04), recrystallization reactor (DI 05), chlorination kettle (DI03), chlorination water washing tank (DI04), drying kettle (L103), distillation column (E101), tank (F102), tank (F103), cyclohexanone distillation column (E102), tank (F104), ethanol distillation column (E103), tank 10 (Fl05); among them, tank (Fl01) is used to store liquid chlorine, tank (Fl02) is used to store previous fraction, tank (Fl03) is used to store chlorinated n-octane, tank (F104) is used to store cyclohexanone, tank (F104) is used to store ethanol; among them, transfer pump (JI01) is connected respectively to chlorination reactor (DI01) and synthesis reactor (DI02), transfer pump (JI03) is connected respectively to drying 15 oven (LI02) and finished product synthetic reactor (DI04); among them, cylinder diameter of tank (Fl 01) is 900-1000 mm.
2. 2-hydroxy-4-octoxybenzophenone production plant, according to claim 1 wherein nominal volume of chlorination reactor (D101) is 800-900 L.
3. 2-hydroxy-4-octoxybenzophenone production plant, according to claim 1
20 wherein heat pipe diameter of condenser (C101) is 0.013-0.014 m.
2018101932 03 Dec 2018
AU2018101932A 2017-12-16 2018-12-03 2-hydroxy-4-octoxybenzophenone production plant Ceased AU2018101932A4 (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
CN2017113479446 2017-12-16
CN201711347944.6A CN108238842A (en) 2017-12-16 2017-12-16 The process units of 2- hydroxyl -4- octyloxybenzophenones

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AU2018101932A4 true AU2018101932A4 (en) 2019-01-31

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AU (1) AU2018101932A4 (en)
GB (1) GB201722082D0 (en)

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CN108238842A (en) 2018-07-03

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