CN208494152U - A kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel - Google Patents

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

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CN208494152U
CN208494152U CN201820799092.8U CN201820799092U CN208494152U CN 208494152 U CN208494152 U CN 208494152U CN 201820799092 U CN201820799092 U CN 201820799092U CN 208494152 U CN208494152 U CN 208494152U
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main body
reactor main
acetylbutyrylcellulose
functional
circulating pump
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CN201820799092.8U
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贾康乐
麦裕良
张�雄
张磊
廖兵
高敏
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Institute of Chemical Engineering of Guangdong Academy of Sciences
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Guangdong Petroleum And Fine Chemical Research Institute
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Abstract

The utility model discloses a kind of multi-functional acetylbutyrylcellulose synthesis reaction vessels, including 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, circulating pump includes inlet and liquid outlet, the inlet of circulating pump and the bottom of reactor main body connect, the liquid outlet of circulating pump and the top of reactor main body connect, the connection of the liquid outlet of liquid distribution device and circulating pump, filter device is located between agitating device and the inlet of circulating pump, agitating device is located between liquid distribution device and filter device.The utility model has the advantages that solid material is difficult to stir when being in activation stage, selecting response uses centrifugal pump to carry out outer loop to reach the mixing purpose of material.When the reaction later period, material viscosity is reduced, and optional agitating paddle is stirred, it can be achieved that efficiently activation and reaction.The utility model relates to field of chemical equipment.

Description

A kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel
Technical field
The utility model relates to field of chemical equipment, in particular to a kind of multi-functional acetylbutyrylcellulose synthetic reaction Kettle.
Background technique
Acetylbutyrylcellulose (cellulose acetate butyrate, abbreviation CAB) is that one kind is widely used in applying Expect the additive of industry, compared to traditional cellulose acetate, soluble range is wider, not only it is 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 units such as washs and dries to operate to obtain final products.
In the prior art, Chinese utility model patent " a kind of acetylbutyrylcellulose mixed ester of high bytyry content and Preparation method (application publication number: CN 104371026, Shen Qing Publication date: 2015.02.25) ", uses temperature for 25~30 Cellulose is activated under the conditions of DEG C, activation time is 12~15h;Document " the heterogeneous synthetic method of acetylbutyrylcellulose (the coatings industry 38.6 (2008) such as yellow color knot: 40-42.) ", use temperature under the conditions of 95 DEG C to cellulose activation, when activation Between be only 2h.Comparison can effectively shorten activation time it is found that improving activation temperature by analysis, improve combined coefficient.It is existing The defect of technology is: reaction raw materials cellulose fibre is longer, is difficult to stir in activation process, and high-temperature activation is due to being heated not Uniformly, it is uneven to easily lead to priming reaction, product structure is caused to have differences.
Utility model content
The technical problem to be solved by the utility model is to provide a kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel, Its priming reaction speed is fast during synthesizing acetylbutyrylcellulose, high-efficient and uniformity coefficient is high, and acetate butyrate can be improved The quality of cellulose products.
A kind of used technical solution to solve above-mentioned technical problem: multi-functional acetylbutyrylcellulose synthetic reaction Kettle including reactor main body, the heating device being located in reactor main body, the agitating device being located in reactor main body, is located at Filter device, the liquid distribution device being located in reactor main body in reactor main body and the circulation 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 top and the bottom of blade of strainer 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 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.
As an improvement, 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.
The utility model has the advantages that
(1) the utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel, have two sets of Matter Transfer sides Case.When in activation stage, solid material is difficult to stir, and selecting response uses centrifugal pump to carry out outer loop to reach material Mix purpose.When the reaction later period, material viscosity is reduced, and optional agitating paddle is stirred, it can be achieved that efficiently activation and reaction.
(2) the utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel, reaction kettle master can not opened Realization activates in the case where body and that reacts is carried out continuously, and avoids the dirt of the separation bring volatile organic matter of activating solution Dye.
(3) the utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel, 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.
Detailed description of the invention
The utility model is described further with reference to the accompanying drawing:
Fig. 1 is the structural schematic diagram of the utility model embodiment;
Fig. 2 is FT-IR (fourier infrared analysis) map of the pilot sample of the utility model embodiment;
Fig. 3 is 1H-NMR (hydrogen nuclear magnetic resonance spectrum analysis) map of the pilot sample of the utility model embodiment;
The noun and label that embodiment and Figure of description are related to include: 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 embodiment
Referring to figs. 1 to 3, a kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel, including reactor main body 3, be located at it is anti- Answer the heating device in kettle 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 and 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 circulation can promote the mixing of solid material by promoting liquid flowing.
In order to be uniformly distributed liquid reactants, liquid distribution device 4 is connect with the liquid outlet of circulating pump 6.
The inlet of solid reactant blocking circulating pump 6, filter device are located at agitating device and circulating pump 6 in order to prevent Between inlet.
In order to promote the reaction of solid-liquid mixture, agitating device is located between liquid distribution device 4 and filter device.When When acetylbutyrylcellulose synthetic reaction proceeds to the later period, the viscosity of reaction mass is reduced, and can be started agitating device, be made solid-liquid Mixed material accelerates reaction, the uniformity coefficient of reaction efficiency and acetylbutyrylcellulose product can be improved, to improve product Quality.
In order to further promote the reaction of solid-liquid mixture, agitating device is agitating paddle 2, and 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, on each agitating shaft also it is settable it is multiple together 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, is stirred 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 At the center of 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 be heated evenly reactor main body 3, 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 utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel, have 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 period, material viscosity is reduced, and agitating paddle 2 can be selected and be stirred, it can be achieved that efficiently activation and reaction.
The utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel, reactor main body 3 can not opened In the case where realize activation and reaction be carried out continuously, avoid the pollution of the separation bring volatile organic matter of activating solution.
The utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel 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.
The utility model proposes multi-functional acetylbutyrylcellulose synthesis reaction vessel production acetylbutyrylcellulose one Kind embodiment: setting the volume that acetic acid is added as AmL, and the volume that butyric acid is added is BmL, from material inlet into reactor main body 3 90g absorbent cotton, AmL acetic acid and BmL butyric acid, conduction oil is added to be flowed by heat conducting oil inlet 5, is flowed out by conduction oil outlet 9, it is thermally conductive Oil temperature is set as 95 DEG C, opens circulating pump 6, circular response 2h, this stage is the activation of cellulose.After activation stage, Continue that 408.6mL butyric anhydride and the 3mL concentrated sulfuric acid is added from material inlet, keep 95 DEG C of thermally conductive oil temperature constant, circulating pump 6 continues 5min is run, circulating pump 6 is then stopped, agitating paddle 2 is opened, is stirred to react 5h;Discharge port 7 is connect with the inlet of circulating pump 6, Reaction mass is released by discharge port 7 after reaction, is produced by sequence of operations such as precipitating, boiling, washing, dryings Product.The structure of sample is analyzed by FT-IR (fourier infrared analysis) and 1H-NMR (hydrogen nuclear magnetic resonance spectrum analysis).
The present embodiment provides three groups of pilot sample experimental datas:
Experimental group 1: being added the volume A=1800mL of acetic acid, and 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: being added the volume A=1200mL of acetic acid, and 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: being added the volume A=300mL of acetic acid, and 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%.
The embodiments of the present invention is explained in detail above in conjunction with attached drawing, but the utility model is not limited to State embodiment, technical field those of ordinary skill within the scope of knowledge, can also do not depart from it is practical Various changes can be made under the premise of novel objective.

Claims (10)

1. a kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel, it is characterised in that: including reactor main body (3), be located at instead Answer the heating device on kettle main body (3), the agitating device being located in reactor main body (3), the mistake being located in reactor main body (3) Device, the liquid distribution device (4) being located in reactor main body (3) and the circulating pump (6) connecting with reactor main body (3) are filtered, The circulating pump (6) includes inlet and liquid outlet, and the inlet of circulating pump (6) connect with the bottom of reactor main body (3), follows The liquid outlet of ring pump (6) is connect with the top of reactor main body (3), and the liquid outlet of liquid distribution device (4) and circulating pump (6) connects Connect, filter device is located between agitating device and the inlet of circulating pump (6), agitating device be located at liquid distribution device (4) with Between filter device.
2. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 1, it is characterised in that: the stirring dress It is set to agitating paddle (2), agitating paddle (2) includes agitating shaft and the blade that is located on agitating shaft, and blade is located at the liquid distribution dress It sets between (4) and filter device, the top of reactor main body (3) is equipped with the motor (1) of driving agitating paddle (2).
3. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 2, it is characterised in that: the filtering dress It is set to strainer (8), the top of strainer (8) and the distance between the bottom of the blade are set as a, 10cm≤a≤20cm.
4. multi-functional acetylbutyrylcellulose synthesis reaction vessel 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. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 2, it is characterised in that: the liquid point The center of cloth apparatus (4) is equipped with channel, and the agitating shaft passes through channel and connect with the blade.
6. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 2, it is characterised in that: the reaction kettle The section of the inner cavity of main body (3) is circle, and the blade is located at the center of the inner cavity of reactor main body (3).
7. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 1, it is characterised in that: the reaction kettle Main body (3) is enamel material.
8. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 1, it is characterised in that: the circulating pump It (6) is corrosion resistant type centrifugal pump.
9. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 1, it is characterised in that: the heating dress It is set to heating jacket, heating jacket is set in the outside of the reactor main body (3).
10. multi-functional acetylbutyrylcellulose synthesis reaction vessel according to claim 9, it is characterised in that: the heating Collet 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.
CN201820799092.8U 2018-05-25 2018-05-25 A kind of multi-functional acetylbutyrylcellulose synthesis reaction vessel Active CN208494152U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108786668A (en) * 2018-05-25 2018-11-13 广东省石油与精细化工研究院 A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose
CN115212832A (en) * 2022-07-21 2022-10-21 江西海瑞天然植物有限公司 Preparation method of butyrate essential oil compound feed additive

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108786668A (en) * 2018-05-25 2018-11-13 广东省石油与精细化工研究院 A kind of multi-functional synthesis reaction vessel and synthetic method of acetylbutyrylcellulose
CN115212832A (en) * 2022-07-21 2022-10-21 江西海瑞天然植物有限公司 Preparation method of butyrate essential oil compound feed additive

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Address after: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318

Patentee after: Institute of chemical engineering, Guangdong Academy of Sciences

Address before: 510665 Guangzhou, Guangdong, Tianhe District Province Road West, No. 318

Patentee before: GUANGDONG RESEARCH INSTITITUTE OF PETROCHEMICAL AND FINE CHEMICAL ENGINEERING

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