CN112851858B - C5 petroleum resin takes off system of urging - Google Patents

C5 petroleum resin takes off system of urging Download PDF

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Publication number
CN112851858B
CN112851858B CN202110040205.2A CN202110040205A CN112851858B CN 112851858 B CN112851858 B CN 112851858B CN 202110040205 A CN202110040205 A CN 202110040205A CN 112851858 B CN112851858 B CN 112851858B
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pipe
petroleum resin
tower
filter
precipitation tower
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CN112851858A (en
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崔广军
鹿伟
袁文培
赵浩哲
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Zibo Luhuahongjin New Material Group Co ltd
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Zibo Luhuahongjin New Material Group Co ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F6/00Post-polymerisation treatments
    • C08F6/02Neutralisation of the polymerisation mass, e.g. killing the catalyst also removal of catalyst residues
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F240/00Copolymers of hydrocarbons and mineral oils, e.g. petroleum resins

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Addition Polymer Or Copolymer, Post-Treatments, Or Chemical Modifications (AREA)

Abstract

The invention provides a C5 petroleum resin de-catalysis system. In the technical scheme, firstly, AlCl is precipitated by alkali liquor 3 In the catalyst process, a heat exchanger is used for avoiding overheating of a system, and a backflow passage is constructed for ensuring that aluminum ions are fully precipitated; filtering C5 petroleum resin containing alkali solution, precipitating in alcohol precipitation tower, and treating with BF 3 After the catalyst is fully precipitated, the catalyst is firstly filtered by a second filter and then sprayed into a washing tower by a distributor; the spray water is fully contacted with C5 petroleum resin containing alkali liquor and methanol to ensure that the alkali liquor, the methanol and the non-precipitated AlCl 3 、BF 3 A homogeneous aqueous phase is formed and removed by stratification to complete the de-catalysis. The invention completes the removal of two Friedel-Crafts catalysts on one process route, simultaneously removes the alkali liquor and the methanol which participate in the reaction, has the advantages of short flow, high removal rate, simple process and the like, and is AlCl 3 ‑BF 3 The application of the composite catalyst in the C5 petroleum resin synthesis process lays a good foundation.

Description

C5 petroleum resin takes off system of urging
Technical Field
The invention relates to the technical field of chemical engineering, in particular to a C5 petroleum resin catalysis removing system.
Background
The C5 petroleum resin is a thermoplastic resin produced by the processes of pretreatment, polymerization, distillation, etc. of the by-product carbon five fraction produced by petroleum cracking. The C5 petroleum resin has good viscosity increasing property, heat resistance, stability, water resistance, acid and alkali resistance, safety and no toxicity, and the tackifying effect of the resin is generally better than that of the C9 resin. The styrene-butadiene rubber has good compatibility with phenolic resin, terpene resin, coumarone resin, natural rubber, synthetic rubber and the like, and particularly has excellent compatibility with styrene-butadiene rubber. The C5 petroleum resin has wide application in products such as pressure-sensitive adhesive, hot-melt adhesive, rubber type adhesive and the like.
At present, the production process of the C5 petroleum resin is similar,comprises the steps of pretreatment of raw materials, polymerization, post-treatment of products, separation of polymer resin, solvent recovery, three-waste treatment and the like. Wherein the polymerization reaction is a core reaction process and is generated by cationic polymerization of C5 fraction under the action of a catalyst. In the prior art, BF is generally adopted 3 Or AlCl 3 And the like Friedel-Crafts catalysts. Wherein, anhydrous AlCl is used 3 When the catalyst is a polymerization catalyst, the catalyst is directly added into a reaction liquid to easily generate implosion and generate a large amount of colloid due to overhigh local temperature, and dicyclopentadiene in the C5 fraction is easily subjected to self-polymerization, so that the softening point of the petroleum resin is reduced, and the chromaticity of the petroleum resin is relatively deep; with BF alone 3 In the case of the catalyst, the obtained petroleum resin has lighter chroma but relatively lower yield and softening point.
In order to solve the above problems, researchers have used toluene as a solvent and AlCl 3 And BF 3 The composite catalyst is compounded according to a certain proportion. Under specific compounding conditions, the catalyst has relatively high yield and softening point, and is helpful for reducing the chroma of the product. However, the technical difficulty of the catalyst removal is brought by the scheme, the conventional catalyst removal process cannot be performed at one time, and if the catalyst removal process is performed separately, the technical problems of long process flow and insufficient catalyst removal exist.
Disclosure of Invention
The invention aims to provide a C5 petroleum resin de-catalysis system aiming at overcoming the technical defects of the prior art, and solves the problem that the conventional de-catalysis system cannot remove AlCl at one time 3 -BF 3 The technical problem of the composite catalyst.
Another technical problem to be solved by the invention is how to fully ensure AlCl 3 -BF 3 The removal rate of the composite catalyst.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
a C5 petroleum resin depyrogenation system comprises an alkali precipitation tower, a heat exchanger, a first primary filter, a cooling jacket, a return pipe, a first secondary filter, an alcohol precipitation tower, a first booster pipe, a second filter, a distributor, a washing tower, a sprayer, a water supply pipe, a second booster pipe and a discharge pipe, wherein the alkali precipitation tower is provided with the heat exchanger, the output end of the alkali precipitation tower is connected to the first primary filter, the first primary filter is provided with the cooling jacket, one output end of the first primary filter is connected to the alkali precipitation tower through the return pipe, the other output end of the first primary filter is connected to the first secondary filter, the output end of the first secondary filter is connected to the alcohol precipitation tower, the alcohol precipitation tower is provided with the first booster pipe, the output end of the alcohol precipitation tower is connected to the second filter, the output end of the second filter is connected to the distributor, the output end of the sprayer is positioned in the washing tower, the top end of the washing tower is fixedly connected with the sprayer, the sprayer is connected with a water supply pipe, the second pressure increasing pipe is connected to the sprayer, and the bottom end of the washing tower is fixedly connected with a discharging pipe.
Preferably, the material distributor further comprises a fan, and the fan is located on the rear side of the output end of the material distributor.
Preferably, the number of the second filters is several, and the several second filters are connected in parallel at the output end of the alcohol precipitation tower.
Preferably, the first pressure increasing pipe and the second pressure increasing pipe are respectively connected to a pressure increasing pump, and the first pressure increasing pipe and the second pressure increasing pipe are respectively connected to a gas filter.
Preferably, an electric heater is disposed outside the alkali precipitation tower, a temperature sensor is disposed inside the alkali precipitation tower, and the temperature sensor and the electric heater are respectively connected to a PLC controller.
In the technical proposal, the alkali precipitation tower is used for supplying C5 petroleum resin crude product and Ca (OH) 2 Or NaOH, thereby causing AlCl 3 Formation of catalyst Al (OH) 3 Precipitating; the heat exchanger is used for accessing refrigerant water and is used for avoiding overhigh temperature of the system; the first primary filter is used for performing primary filtering; the cooling jacket is used for further cooling the feed liquid before the feed liquid enters the alcohol precipitation tower; the reflux pipe is provided with a pump body which can be selectively opened according to actual conditions, so that the feed liquid is repeatedly contacted with the alkali liquor, and the problem of insufficient aluminum ion precipitation is avoided; the first primary filter has a smaller pore size than the first primary filter, and is subjected to two-stage filtration to obtain Al (OH) 3 Fully intercepting; the crude product of C5 petroleum resin containing alkali liquor enters an alcohol precipitation tower, BF 3 The catalyst reacts with methanol to generate oil insoluble substances;the second filter is used for filtering the precipitate; the first booster duct is used for providing power for the filtering process; the distributor is used for spraying the crude C5 petroleum resin product containing alkali liquor and methanol into the washing tower to make it contact with spray water with large surface area, the spray water forms uniform water phase with the alkali liquor and methanol, and makes possible AlCl which is not precipitated 3 、BF 3 Dissolving the mixture in the solvent, and finally removing the water phase through layering to finish the de-catalysis; the sprayer and the water supply pipe are used for supplying spraying water; the second pressure increasing pipe can be used for increasing the initial speed of the spray water; the discharge pipe is used for respectively discharging the water phase and the oil phase after layering.
The invention provides a C5 petroleum resin de-catalysis system. In the technical scheme, firstly, AlCl is precipitated by using alkali liquor 3 In the catalyst process, a heat exchanger is used for avoiding overheating of a system, and a backflow passage is constructed for ensuring that aluminum ions are fully precipitated; filtering C5 petroleum resin containing alkali solution, precipitating in alcohol precipitation tower, and treating with BF 3 After the catalyst is fully precipitated, the catalyst is firstly filtered by a second filter and then sprayed into a washing tower by a distributor; the spray water is fully contacted with C5 petroleum resin containing alkali liquor and methanol to ensure that the alkali liquor, the methanol and the non-precipitated AlCl 3 、BF 3 A homogeneous aqueous phase is formed and removed by stratification to complete the de-catalysis. The invention completes the removal of two Friedel-Crafts catalysts on one process route, simultaneously removes the alkali liquor and the methanol which participate in the reaction, has the advantages of short flow, high removal rate, simple process and the like, and is AlCl 3 -BF 3 The application of the composite catalyst in the C5 petroleum resin synthesis process lays a good foundation.
Drawings
FIG. 1 is a schematic structural view of the present invention;
in the figure:
1. an alkali precipitation tower 2, a heat exchanger 3, a first primary filter 4 and a cooling jacket
5. A return pipe 6, a first secondary filter 7, an alcohol precipitation tower 8 and a first pressure increasing pipe
9. A second filter 10, a distributor 11, a washing tower 12 and a fan
13. A sprayer 14, a water supply pipe 15, a second pressure increasing pipe 16 and a discharge pipe.
Detailed Description
Hereinafter, specific embodiments of the present invention will be described in detail. Well-known structures or functions may not be described in detail in the following embodiments in order to avoid unnecessarily obscuring the details. Approximating language, as used herein in the following examples, may be applied to represent quantitative representations that could permissibly vary in number without resulting in a change in the basic function. Unless defined otherwise, technical and scientific terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
Example 1
A C5 petroleum resin de-catalysis system is shown in figure 1 and comprises an alkali precipitation tower 1, a heat exchanger 2, a first primary filter 3, a cooling jacket 4, a return pipe 5, a first secondary filter 6, an alcohol precipitation tower 7, a first pressure increasing pipe 8, a second filter 9, a distributor 10, a washing tower 11, a sprayer 13, a water supply pipe 14, a second pressure increasing pipe 15 and a discharge pipe 16, wherein the heat exchanger 2 is arranged on the alkali precipitation tower 1, the output end of the alkali precipitation tower 1 is connected to the first primary filter 3, the cooling jacket 4 is arranged on the first primary filter 3, one output end of the first primary filter 3 is connected to the alkali precipitation tower 1 through the return pipe 5, the other output end of the first primary filter 3 is connected to the first secondary filter 6, the output end of the first secondary filter 6 is connected to the alcohol precipitation tower 7, the first pressure increasing pipe 8 is arranged on the alcohol precipitation tower 7, the output end of the alcohol precipitation tower 7 is connected to the second alcohol precipitation filter 9, the output end of the second filter 9 is connected to a distributor 10, the output end of the distributor 10 is located in a washing tower 11, a sprayer 13 is fixedly connected to the top end of the washing tower 11, a water supply pipe 14 is connected to the sprayer 13, a second pressure increasing pipe 15 is connected to the sprayer 13, and a discharging pipe 16 is fixedly connected to the bottom end of the washing tower 11.
The system has the following structural characteristics: the alkali precipitation tower 1 is used for supplying C5 petroleum resin crude product and Ca (OH) 2 Or NaOH, thereby enabling AlCl 3 Formation of catalyst Al (OH) 3 Precipitating; the heat exchanger 2 is used for connecting refrigerant water and avoiding a systemThe temperature is too high; the first primary filter 3 is used for performing primary filtering; the cooling jacket 4 is used for further cooling the feed liquid before the feed liquid enters the alcohol precipitation tower 7; the reflux pipe 5 is provided with a pump body which can be selectively opened according to actual conditions, so that the feed liquid is repeatedly contacted with the alkali liquor, and the problem of insufficient aluminum ion precipitation is avoided; the first secondary filter 6 having a pore size smaller than that of the first primary filter 3, and filtering the resulting mixture in two stages to remove Al (OH) 3 Fully intercepting; the crude product of C5 petroleum resin containing alkali liquor enters an alcohol precipitation tower 7, BF 3 The catalyst reacts with methanol to generate oil insoluble substances; a second filter 8 for filtering the precipitate; the first pressure inlet 9 is used to power this filtration process; the distributor 10 is used to spray the crude C5 petroleum resin product containing lye and methanol into the washing column 11, to bring it into contact with the spray water over a large surface area, the spray water forming a homogeneous aqueous phase with the lye and methanol and causing AlCl, which may be present and which has not been precipitated, to form a precipitate 3 、BF 3 Dissolving the mixture in the solvent, and finally removing the water phase through layering to finish the de-catalysis; the shower 13 and the water supply pipe 14 are used to supply shower water; the second booster pipe 15 may be used to increase the initial velocity of the shower water; the discharge pipe 16 is used to discharge the aqueous phase and the oil phase, respectively, after the layering.
Example 2
A C5 petroleum resin de-catalysis system is shown in figure 1 and comprises an alkali precipitation tower 1, a heat exchanger 2, a first primary filter 3, a cooling jacket 4, a return pipe 5, a first secondary filter 6, an alcohol precipitation tower 7, a first pressure increasing pipe 8, a second filter 9, a distributor 10, a washing tower 11, a sprayer 13, a water supply pipe 14, a second pressure increasing pipe 15 and a discharge pipe 16, wherein the heat exchanger 2 is arranged on the alkali precipitation tower 1, the output end of the alkali precipitation tower 1 is connected to the first primary filter 3, the cooling jacket 4 is arranged on the first primary filter 3, one output end of the first primary filter 3 is connected to the alkali precipitation tower 1 through the return pipe 5, the other output end of the first primary filter 3 is connected to the first secondary filter 6, the output end of the first secondary filter 6 is connected to the alcohol precipitation tower 7, the first pressure increasing pipe 8 is arranged on the alcohol precipitation tower 7, the output end of the alcohol precipitation tower 7 is connected to the second alcohol precipitation filter 9, the output end of the second filter 9 is connected to a distributor 10, the output end of the distributor 10 is located in a washing tower 11, a sprayer 13 is fixedly connected to the top end of the washing tower 11, a water supply pipe 14 is connected to the sprayer 13, a second pressure increasing pipe 15 is connected to the sprayer 13, and a discharging pipe 16 is fixedly connected to the bottom end of the washing tower 11. Meanwhile, the device also comprises a fan 12, wherein the fan 12 is positioned at the rear side of the output end of the distributing device 10. The number of the second filters 9 is several, and the several second filters 9 are connected in parallel at the output end of the alcohol precipitation tower 7. The first pressure increasing pipe 8 and the second pressure increasing pipe 15 are connected to a pressure increasing pump, respectively, and a gas filter is connected to the first pressure increasing pipe 8 and the second pressure increasing pipe 15, respectively. An electric heater is arranged outside the alkali precipitation tower 1, a temperature sensor is arranged inside the alkali precipitation tower 1, and the temperature sensor and the electric heater are respectively connected to a PLC (programmable logic controller).
The embodiments of the present invention have been described in detail, but the description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. Any modification, equivalent replacement, and improvement made within the scope of the application of the present invention should be included in the protection scope of the present invention.

Claims (5)

1. A C5 petroleum resin catalysis removal system is characterized by comprising an alkali precipitation tower (1), a heat exchanger (2), a first primary filter (3), a cooling jacket (4), a return pipe (5), a first secondary filter (6), an alcohol precipitation tower (7), a first booster pipe (8), a second filter (9), a distributor (10), a washing tower (11), a sprayer (13), a water supply pipe (14), a second booster pipe (15) and a material discharge pipe (16), wherein the alkali precipitation tower (1) is provided with the heat exchanger (2), the output end of the alkali precipitation tower (1) is connected to the first primary filter (3), the first primary filter (3) is provided with the cooling jacket (4), one path of output end of the first primary filter (3) is connected to the alkali precipitation tower (1) through the return pipe (5), the other path of output end of the first primary filter (3) is connected to the first secondary filter (6), the output of first secondary filter (6) is connected to alcohol precipitation tower (7), be provided with first booster pipe (8) on alcohol precipitation tower (7), the output of alcohol precipitation tower (7) is connected to second filter (9), the output of second filter (9) is connected to distributing device (10), the output of distributing device (10) is located washing tower (11), top fixedly connected with spray thrower (13) at washing tower (11), be connected with delivery pipe (14) on spray thrower (13), second booster pipe (15) are connected to spray thrower (13), arrange material pipe (16) at the bottom fixedly connected with of washing tower (11).
2. The C5 petroleum resin depyrogenation system according to claim 1, further comprising a fan (12), wherein the fan (12) is located at the rear side of the output end of the distributor (10).
3. The C5 petroleum resin depyrogenation system according to claim 1, wherein the number of the second filters (9) is several, and the several second filters (9) are connected in parallel at the output end of the alcohol precipitation tower (7).
4. The C5 petroleum resin dehydrogenation system according to claim 1, wherein the first pressure increasing pipe (8) and the second pressure increasing pipe (15) are respectively connected to a pressure increasing pump, and a gas filter is respectively connected to the first pressure increasing pipe (8) and the second pressure increasing pipe (15).
5. The C5 petroleum resin dehydrogenation catalyst system according to claim 1, wherein an electric heater is installed outside the alkali precipitation tower (1), a temperature sensor is installed inside the alkali precipitation tower (1), and the temperature sensor and the electric heater are respectively connected to a PLC controller.
CN202110040205.2A 2021-01-13 2021-01-13 C5 petroleum resin takes off system of urging Active CN112851858B (en)

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Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1944484A (en) * 2006-10-09 2007-04-11 中国石油兰州石油化工公司 Method for removing aluminum trichloride and purifying products in C5 petroleum resin production process
CN102086251A (en) * 2010-12-27 2011-06-08 淄博鲁华泓锦化工股份有限公司 Continuous alkali washing method of C5 petroleum resin
CN102382260A (en) * 2011-08-22 2012-03-21 天津市兴源化工有限公司 Method for removing BF3 catalyst in petroleum resin production
CN102659984A (en) * 2012-06-07 2012-09-12 抚顺齐隆化工有限公司 Method for removing aluminium trichloride catalyst in petroleum resin in combination with waster cleaning and dry cleaning
CN102757530A (en) * 2012-06-27 2012-10-31 宁波职业技术学院 Preparation method of light-color cold polymerized C9 petroleum resin
CN102899080A (en) * 2011-07-24 2013-01-30 天津海阔天平化工有限公司 Production method for preparing aromatic hydrocarbon solvent oil by using C9 fraction
CN105418848A (en) * 2015-12-09 2016-03-23 宁波甬华树脂有限公司 Method for catalyzed preparation of C5 petroleum resin by utilizing boron trifluoride
CN105542080A (en) * 2015-12-31 2016-05-04 广东工业大学 Method for preparing petroleum resin in microreactor
CN111704684A (en) * 2020-07-17 2020-09-25 恒河材料科技股份有限公司 Method for modifying C5/C9 copolymer resin by using peracetic acid

Patent Citations (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1944484A (en) * 2006-10-09 2007-04-11 中国石油兰州石油化工公司 Method for removing aluminum trichloride and purifying products in C5 petroleum resin production process
CN102086251A (en) * 2010-12-27 2011-06-08 淄博鲁华泓锦化工股份有限公司 Continuous alkali washing method of C5 petroleum resin
CN102899080A (en) * 2011-07-24 2013-01-30 天津海阔天平化工有限公司 Production method for preparing aromatic hydrocarbon solvent oil by using C9 fraction
CN102382260A (en) * 2011-08-22 2012-03-21 天津市兴源化工有限公司 Method for removing BF3 catalyst in petroleum resin production
CN102659984A (en) * 2012-06-07 2012-09-12 抚顺齐隆化工有限公司 Method for removing aluminium trichloride catalyst in petroleum resin in combination with waster cleaning and dry cleaning
CN102757530A (en) * 2012-06-27 2012-10-31 宁波职业技术学院 Preparation method of light-color cold polymerized C9 petroleum resin
CN105418848A (en) * 2015-12-09 2016-03-23 宁波甬华树脂有限公司 Method for catalyzed preparation of C5 petroleum resin by utilizing boron trifluoride
CN105542080A (en) * 2015-12-31 2016-05-04 广东工业大学 Method for preparing petroleum resin in microreactor
CN111704684A (en) * 2020-07-17 2020-09-25 恒河材料科技股份有限公司 Method for modifying C5/C9 copolymer resin by using peracetic acid

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