CN108786668A - A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose - Google Patents

A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose Download PDF

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Publication number
CN108786668A
CN108786668A CN201810520771.1A CN201810520771A CN108786668A CN 108786668 A CN108786668 A CN 108786668A CN 201810520771 A CN201810520771 A CN 201810520771A CN 108786668 A CN108786668 A CN 108786668A
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China
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main body
acetylbutyrylcellulose
reactor main
reaction vessel
synthesis reaction
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Pending
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CN201810520771.1A
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Chinese (zh)
Inventor
贾康乐
麦裕良
张�雄
张磊
廖兵
高敏
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Guangdong Petroleum And Fine Chemical Research Institute
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Guangdong Petroleum And Fine Chemical Research Institute
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Priority to CN201810520771.1A priority Critical patent/CN108786668A/en
Publication of CN108786668A publication Critical patent/CN108786668A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/087Heating or cooling the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/08Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles
    • B01J8/10Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with moving particles moved by stirrers or by rotary drums or rotary receptacles or endless belts
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00168Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00176Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles outside the reactor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00008Controlling the process
    • B01J2208/00017Controlling the temperature
    • B01J2208/00106Controlling the temperature by indirect heat exchange
    • B01J2208/00168Controlling the temperature by indirect heat exchange with heat exchange elements outside the bed of solid particles
    • B01J2208/00212Plates; Jackets; Cylinders
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00823Mixing elements
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2208/00Processes carried out in the presence of solid particles; Reactors therefor
    • B01J2208/00796Details of the reactor or of the particulate material
    • B01J2208/00823Mixing elements
    • B01J2208/00858Moving elements
    • B01J2208/00867Moving elements inside the bed, e.g. rotary mixer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Polysaccharides And Polysaccharide Derivatives (AREA)

Abstract

The invention discloses the multi-functional synthesis reaction vessel and synthetic method of a kind of acetylbutyrylcellulose, this multi-functional synthesis reaction vessel includes reactor main body, the agitating device being located in reactor main body, the filter device being located in reactor main body, the liquid distribution device being located in reactor main body and the circulating pump being connect with reactor main body.A kind of method synthesizing acetylbutyrylcellulose using the reaction kettle is also disclosed that simultaneously.Advantageous effect:Using the reaction kettle synthesis acetylbutyrylcellulose of the present invention, it can be achieved that efficiently activation and reaction;Being carried out continuously for activation and reaction can be realized in the case where not opening reactor main body, avoid the pollution for the volatile organic matter that the separation of activating solution is brought;By being transformed to pipeline, can carry out the precipitating of product, boiling, the sequence of operations such as be filtered, washed, it can be achieved that a tractor serves several purposes purpose.The present invention relates to field of chemical equipment.

Description

A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose
Technical field
The present invention relates to field of chemical equipment, more particularly to the multi-functional synthesis reaction vessel of a kind of acetylbutyrylcellulose.
Background technology
Acetylbutyrylcellulose (cellulose acetate butyrate, abbreviation CAB) is that one kind is widely used in applying To expect the additive of industry, compares traditional cellulose acetate, soluble range is wider, is not only dissolved in intensive polar solvent, The acetylbutyrylcellulose of high butyl ester content even dissolves in alcohols solvent.Therefore, it is widely used in woodwork coating, plastics apply Material etc. applies in item, has the function of to improve coating mobility, levelability, outdoor durable, pigment directionality and flexibility etc..
The synthetic route of acetylbutyrylcellulose is as follows:Cellulose is activated under certain condition first, to destroy it Hydrogen bond;Esterifying agent is added and catalyst carries out esterification;Precipitating agent is added after reaction, precipitating is carried out to product;Product is by washing It the unit operations such as washs and dries and obtain final products.
In the prior art, Chinese invention patent " a kind of the acetylbutyrylcellulose mixed ester and its system of high bytyry content Preparation Method (application publication number:CN 104371026A, Shen Qing Publication date:2015.02.25) ", use temperature for 25~30 DEG C Under the conditions of cellulose is activated, soak time be 12~15h;" the heterogeneous synthetic method of acetylbutyrylcellulose is (yellow for document The coatings industries 38.6 (2008) such as coloured silk knot:40-42.) ", use temperature under the conditions of 95 DEG C to cellulose activation, soak time Only 2h.Comparison can effectively shorten soak time it is found that improving activation temperature by analysis, improve combined coefficient.Existing skill The defect of art is:Reaction raw materials cellulose fibre is longer, is difficult to stir in activation process, high-temperature activation is due to uneven heating Even, it is uneven to easily lead to priming reaction, and product structure is caused to have differences.
Invention content
Technical problem to be solved by the invention is to provide a kind of multi-functional synthesis reaction vessel of acetylbutyrylcellulose and Synthetic method, its priming reaction speed is fast during synthesizing acetylbutyrylcellulose, efficient and uniformity coefficient is high, can be improved The quality of acetylbutyrylcellulose product.
Used technical solution to solve above-mentioned technical problem:A kind of multi-functional synthetic reaction of acetylbutyrylcellulose Kettle, including reactor main body, be located in reactor main body heating device, be located in reactor main body agitating device, be located at Filter device, the liquid distribution device being located in reactor main body in reactor main body and the cycle being connect with reactor main body Pump, circulating pump include inlet and liquid outlet, and the inlet of circulating pump and the bottom of reactor main body connect, and circulating pump goes out liquid Mouth is connect with the top of reactor main body, and the liquid outlet connection of liquid distribution device and circulating pump, filter device is located at stirring dress It sets between the inlet of circulating pump, agitating device is located between liquid distribution device and filter device.
As an improvement, agitating device is agitating paddle, agitating paddle includes agitating shaft and the blade that is located on agitating shaft, and blade is set Between liquid distribution device and filter device, the top of reactor main body is equipped with the motor of driving agitating paddle.
As an improvement, filter device is strainer, the distance between the top of strainer and the bottom of blade are set as a, 10cm≤a ≤20cm。
As an improvement, reactor main body is equipped with feeding port, feeding port is located between liquid distribution device and blade.
As an improvement, the center of liquid distribution device is equipped with channel, agitating shaft passes through channel and is connect with blade.
As an improvement, the section of the inner cavity of reactor main body is circle, blade is located at the center of the inner cavity of reactor main body.
As an improvement, reactor main body is enamel material, circulating pump is corrosion resistant type centrifugal pump.
As an improvement, heating device is heating jacket, heating jacket is set in the outside of reactor main body.
As an improvement, heating jacket includes heat conducting oil inlet and conduction oil outlet, heat conducting oil inlet is located at heating jacket Lower part, conduction oil outlet are located at the top of heating jacket.
A kind of synthetic method of acetylbutyrylcellulose is using above-mentioned multi-functional synthesis reaction vessel synthesis acetate butyrate Cellulose.
Advantageous effect:
(1) the multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention has two sets of Matter Transfer schemes. When in activation stage, solid material is difficult to stir, and selecting response uses centrifugal pump to carry out outer loop to reach the mixed of material Close purpose.When the reaction later stage, material viscosity reduces, and optional agitating paddle is stirred, it can be achieved that efficiently activation and reaction.
(2) the multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention can not open reactor main body In the case of realize being carried out continuously for activation and reaction, avoid the pollution for the volatile organic matter that the separation of activating solution is brought.
(3) the multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention can by being transformed to pipeline Carry out the precipitating of product, boiling, the sequence of operations such as be filtered, washed, it can be achieved that a tractor serves several purposes purpose.
Description of the drawings
Following further describes the present invention with reference to the drawings:
Fig. 1 is the structural schematic diagram of the embodiment of the present invention;
Fig. 2 is FT-IR (fourier infrared analysis) collection of illustrative plates of the pilot sample of the embodiment of the present invention;
Fig. 3 is 1H-NMR (hydrogen nuclear magnetic resonance spectrum analysis) collection of illustrative plates of the pilot sample of the embodiment of the present invention;
The noun that embodiment is related to Figure of description includes with label:Motor 1, agitating paddle 2, reactor main body 3, liquid Distribution apparatus 4, heat conducting oil inlet 5, circulating pump 6, discharge port 7, strainer 8, conduction oil outlet 9, feeding port 10.
Specific implementation mode
Referring to figs. 1 to 3, a kind of multi-functional synthesis reaction vessel of acetylbutyrylcellulose, including reactor main body 3, be located at Heating device in reactor main body 3, the agitating device being located in reactor main body 3, the filtering being located in reactor main body 3 dress The liquid distribution device 4 set, being located in reactor main body 3 and the circulating pump 6 being connect with reactor main body 3.
In order to promote the reaction of solid material, circulating pump 6 includes inlet and liquid outlet, the inlet of circulating pump 6 with it is anti- The bottom of kettle main body 3 is answered to connect, the liquid outlet of circulating pump 6 is connect with the top of reactor main body 3.When acetylbutyrylcellulose closes When at reaction in activation stage, reaction mass is mainly solid, and solid material is difficult to stir, and is carried out using circulating pump 6 outer Portion's cycle can promote the mixing of solid material by promoting liquid flowing.
In order to make liquid reactants be uniformly distributed, liquid distribution device 4 is connect with the liquid outlet of circulating pump 6.
Solid reactant blocks the inlet of circulating pump 6 in order to prevent, and filter device is located at agitating device and circulating pump 6 Between inlet.
In order to promote the reaction of solid-liquid mixture, agitating device to be located between liquid distribution device 4 and filter device.When When acetylbutyrylcellulose synthetic reaction proceeds to the later stage, the viscosity of reaction mass reduces, and can start agitating device, make solid-liquid Mixed material accelerates reaction, the uniformity coefficient of reaction efficiency and acetylbutyrylcellulose product can be improved, to improve product Quality.
It is agitating paddle 2 to further promote the reaction of solid-liquid mixture, agitating device, agitating paddle 2 includes agitating shaft With the blade being located on agitating shaft, blade is located between liquid distribution device 4 and filter device, and the top of reactor main body 3 is set There is the motor 1 of driving agitating paddle 2.Agitating device can also include multiple agitating shafts, can also be arranged on each agitating shaft multiple same The blade of axis.Agitating device can also be stirring rod.
Solid material is stacked on blade in order to prevent, and filter device is strainer 8, the top of strainer 8 and the bottom of blade The distance between be set as a, 10cm≤a≤20cm.
For the ease of adding reaction mass, reactor main body 3 is equipped with feeding port 10, and feeding port 10 is located at liquid distribution dress It sets between 4 and blade.
Agitating shaft is interfered with liquid distribution device 4 in order to prevent, and the center of liquid distribution device 4 is equipped with channel, stirs Axis is mixed across channel and is connect with blade.
For the uniformity coefficient of further reaction mass mixing, the section of the inner cavity of reactor main body 3 is circle, and blade is set Center in the inner cavity of reactor main body 3.
In order to keep reactor main body 3 corrosion-resistant and convenient for cleaning, reactor main body 3 is enamel material.
In order to keep circulating pump 6 corrosion-resistant and improve the cycle efficieny of liquid material, circulating pump 6 is corrosion resistant type centrifugal pump.
In order to make reactor main body 3 be heated evenly, heating device is heating jacket, and heating jacket is set in reactor main body 3 outside.
In order to improve the heat distribution situation of reaction system, heating jacket includes heat conducting oil inlet 5 and conduction oil outlet 9, Heat conducting oil inlet 5 is located at the lower part of heating jacket, and conduction oil outlet 9 is located at the top of heating jacket.
The multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention has two sets of Matter Transfer schemes.Place When activation stage, solid material is difficult to stir, and selecting response uses centrifugal pump to carry out outer loop to reach the mixing of material Purpose.When the reaction later stage, material viscosity reduces, and agitating paddle 2 can be selected and be stirred, it can be achieved that efficiently activation and reaction.
The multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention can not open reactor main body 3 In the case of realize being carried out continuously for activation and reaction, avoid the pollution for the volatile organic matter that the separation of activating solution is brought.
The multi-functional synthesis reaction vessel of acetylbutyrylcellulose proposed by the present invention can be by being transformed to pipeline The precipitating of row product, boiling, the sequence of operations such as be filtered, washed, it can be achieved that a tractor serves several purposes purpose.
One kind of the multi-functional synthesis reaction vessel production acetylbutyrylcellulose of acetylbutyrylcellulose proposed by the present invention Embodiment:90g absorbent cotton, the acetic acid that volume is A and the butyric acid that volume is B is added into reactor main body 3 from material inlet, leads Deep fat is flowed by heat conducting oil inlet 5, is flowed out by conduction oil outlet 9, and conduction oil temperature setting is 95 DEG C, open the circulation pump 6, cycle 2h is reacted, this stage is the activation of cellulose.After activation stage, continue from material inlet be added 408.6mL butyric anhydrides and The 3mL concentrated sulfuric acids keep 95 DEG C of heat conduction oil temperature constant, and circulating pump 6 continues to run with 5min, then stop circulating pump 6, open stirring Paddle 2, is stirred to react 5h;Discharge port 7 is connect with the inlet of circulating pump 6, after reaction puts reaction mass by discharge port 7 Go out, product is obtained by sequence of operations such as precipitating, boiling, washing, dryings.The structure of sample is by FT-IR (fourier infrareds point Analysis) and 1H-NMR (hydrogen nuclear magnetic resonance spectrum analysis) analyzed.
The present embodiment provides three groups of pilot sample experimental datas:
Experimental group 1:The volume A=1800mL of acetic acid is added, the volume B=600mL of butyric acid is added.Reference Fig. 2 to 3, by FT-IR and 1H-NMR quantitative analysis results show:Acetyl content 38.06%, bytyry content 14.49%.
Experimental group 2:The volume A=1200mL of acetic acid is added, the volume B=1200mL of butyric acid is added.Reference Fig. 2 to 3, by FT-IR and 1H-NMR quantitative analysis results show:Acetyl content 29.36%, bytyry content 25.10%.
Experimental group 3:The volume A=300mL of acetic acid is added, the volume B=2100mL of butyric acid is added.Reference Fig. 2 to 3, by FT-IR and 1H-NMR quantitative analysis results show:Acetyl content 9.50%, bytyry content 50.10%.
Embodiments of the present invention are explained in detail above in conjunction with attached drawing, but the present invention is not limited to above-mentioned embodiment party Formula, technical field those of ordinary skill within the scope of knowledge, can also be before not departing from present inventive concept Put that various changes can be made.

Claims (10)

1. a kind of multi-functional synthesis reaction vessel of acetylbutyrylcellulose, it is characterised in that:Including reactor main body (3), it is located at Heating device in reactor main body (3), is located in reactor main body (3) agitating device being located in reactor main body (3) Filter device, the liquid distribution device (4) being located in reactor main body (3) and the circulating pump being connect with reactor main body (3) (6), the circulating pump (6) includes inlet and liquid outlet, and the inlet of circulating pump (6) connects with the bottom of reactor main body (3) It connects, the liquid outlet of circulating pump (6) is connect with the top of reactor main body (3), and liquid distribution device (4) goes out with circulating pump (6) Liquid mouth connects, and filter device is located between agitating device and the inlet of circulating pump (6), and agitating device is located at liquid distribution device (4) between filter device.
2. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 1, it is characterised in that:The stirring Device is agitating paddle (2), and agitating paddle (2) includes agitating shaft and the blade that is located on agitating shaft, and blade is located at the liquid distribution For device (4) between filter device, the top of reactor main body (3) is equipped with the motor (1) of driving agitating paddle (2).
3. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 2, it is characterised in that:The filtering Device is strainer (8), and the top of strainer (8) is set as a, 10cm≤a≤20cm with the distance between the bottom of the blade.
4. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 2, it is characterised in that:The reaction Kettle main body (3) is equipped with feeding port (10), and feeding port (10) is located between the liquid distribution device (4) and the blade.
5. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 2, it is characterised in that:The liquid The center of distribution apparatus (4) is equipped with channel, and the agitating shaft passes through channel and connect with the blade.
6. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 2, it is characterised in that:The reaction The section of the inner cavity of kettle main body (3) is circle, and the blade is located at the center of the inner cavity of reactor main body (3).
7. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 1, it is characterised in that:The reaction Kettle main body (3) is enamel material, and the circulating pump (6) is corrosion resistant type centrifugal pump.
8. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 1, it is characterised in that:The heating Device is heating jacket, and heating jacket is set in the outside of the reactor main body (3).
9. the multi-functional synthesis reaction vessel of acetylbutyrylcellulose according to claim 8, it is characterised in that:The heating Chuck includes heat conducting oil inlet (5) and conduction oil outlet (9), and heat conducting oil inlet (5) is located at the lower part of heating jacket, and conduction oil goes out Mouth (9) is located at the top of heating jacket.
10. a kind of synthetic method of acetylbutyrylcellulose, it is characterised in that:Using described in any one of claim 1-9 described The multi-functional synthesis reaction vessel of acetylbutyrylcellulose synthesizes acetylbutyrylcellulose.
CN201810520771.1A 2018-05-25 2018-05-25 A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose Pending CN108786668A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115140564A (en) * 2022-05-13 2022-10-04 南京杰亚挤出装备有限公司 Continuous production line for separating polyester cotton by alcoholysis method

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070100126A1 (en) * 2003-05-08 2007-05-03 China Petroleum & Chemical Corporation Device for reaction or separation and a continuous esterification process using the device
CN102898530A (en) * 2012-09-13 2013-01-30 无锡市凯利药业有限公司 Preparation method for cellulose acetate-butyrate
CN203935841U (en) * 2014-06-23 2014-11-12 湖州纯一生物科技有限公司 A kind of efficient circulation reactor
CN206492492U (en) * 2017-01-17 2017-09-15 张家港南光化工有限公司 Outer circulation compartment system applied to esterification
CN208494152U (en) * 2018-05-25 2019-02-15 广东省石油与精细化工研究院 A kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20070100126A1 (en) * 2003-05-08 2007-05-03 China Petroleum & Chemical Corporation Device for reaction or separation and a continuous esterification process using the device
CN102898530A (en) * 2012-09-13 2013-01-30 无锡市凯利药业有限公司 Preparation method for cellulose acetate-butyrate
CN203935841U (en) * 2014-06-23 2014-11-12 湖州纯一生物科技有限公司 A kind of efficient circulation reactor
CN206492492U (en) * 2017-01-17 2017-09-15 张家港南光化工有限公司 Outer circulation compartment system applied to esterification
CN208494152U (en) * 2018-05-25 2019-02-15 广东省石油与精细化工研究院 A kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115140564A (en) * 2022-05-13 2022-10-04 南京杰亚挤出装备有限公司 Continuous production line for separating polyester cotton by alcoholysis method
CN115140564B (en) * 2022-05-13 2024-06-18 南京杰亚挤出装备有限公司 Continuous production line for separating polyester cotton by alcoholysis method

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