CN203474699U - Rectification type esterification reaction system for polycarboxylate water reducer - Google Patents

Rectification type esterification reaction system for polycarboxylate water reducer Download PDF

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Publication number
CN203474699U
CN203474699U CN201320493218.6U CN201320493218U CN203474699U CN 203474699 U CN203474699 U CN 203474699U CN 201320493218 U CN201320493218 U CN 201320493218U CN 203474699 U CN203474699 U CN 203474699U
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China
Prior art keywords
condenser
rectifying tower
rectifying
esterification
refrigerant
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Expired - Fee Related
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CN201320493218.6U
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Chinese (zh)
Inventor
亓建设
吴振华
李宏石
孙燕杰
时军祥
何伟
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SHANDONG LAIWU CITY WENHE CHEMICAL CO Ltd
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SHANDONG LAIWU CITY WENHE CHEMICAL CO Ltd
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Abstract

The utility model relates to a rectification type esterification reaction system for polycarboxylate water reducer, belonging to the field of production of polycarboxylate water reducer. The rectification type esterification reaction system comprises an esterification reaction kettle, a rectifying tower, a condenser and a liquid receiver, wherein the bottom end of the rectifying tower is communicated with the esterification reaction kettle through a pipeline, a rectifying tower gas outlet is formed in the top of the rectifying tower, the bottom end of the condenser is communicated with the liquid receiver through the pipeline, a condenser gas inlet is formed in the top of the condenser, the rectifying tower gas outlet is communicated with the condenser gas inlet through the pipeline, and a final gas outlet is formed in the tail end of the system. Without using solvents and under the condition of low acid-alcohol ratio, the rectification type esterification reaction system realizes high esterification rate, shortens esterification time, is simple and easy to operate, and does not have so many complex equipment.

Description

A kind of polycarboxylate water-reducer rectifying formula esterification system
Technical field
The utility model relates to a kind of by rectifying separation moisture, the conversion unit of high-level efficiency esterification, and specifically a kind of polycarboxylate water-reducer rectifying formula esterification system, belongs to polycarboxylate water-reducer production field.
Background technology
Acid alcohol esterification is the synthetic important step of high performance water reducing agent of polyocarboxy acid, that unsaturated acid and polyoxyethylene ether alcohol, under catalyst action, esterification is occurred to, if the hydropexis that reaction generates, in reaction system the inside, can hinder to positive reaction direction and carry out, expect high esterification yield, reaction times can be very long, owing to there is undersaturated pair of key, esterification time is longer, and two keys more easily destroy, so try every possible means, moisture is extracted, reaction could be fast thoroughly.
In order to try to achieve the domestic and international producer of higher esterification yield, there are two kinds of modes, the one, at esterification process, adopt solvent method, solvent cycle is used, and final evaporation goes out remaining solvent, and solvent method is very uneconomical, also exists and pollutes.The 2nd, do not use solvent, acid and alcohol heat in esterifying kettle, the method of the moisture that negative pressure extraction produces, reaches esterification object, but when negative pressure extraction moisture, the unsaturated acid of extracting out is also a lot, and concentration is higher, thus usually take to improve the ratio of acid alcohol, or simply add a part of unsaturated acid in the esterification process later stage, virtually cause unnecessary trouble and waste, and the time is long, two key retention rates are low.
Utility model content
The purpose of this utility model is to provide a kind of polycarboxylate water-reducer rectifying formula esterification system, and this system has solved the problem that the acid alcohol direct esterification time is long, esterification yield is low; Also solved the pollution that solvent method brings in the past.
The technical scheme in the invention for solving the technical problem is: a kind of polycarboxylate water-reducer rectifying formula esterification system, comprises reaction kettle of the esterification, rectifying tower, condenser and liquid receiver; Rectifying tower bottom is connected by pipeline with reaction kettle of the esterification, and rectifying tower top is provided with rectifying tower pneumatic outlet; Condenser bottom is connected by pipeline with liquid receiver, and condenser top is provided with condenser gas feed; Between rectifying tower pneumatic outlet and condenser gas feed, by pipeline, be connected, at the terminal portions of system, be also provided with final pneumatic outlet.
Described rectifying tower lower part is rectifying column, and the inside of rectifying column is provided with filler, and rectifying tower upper part is fractionator, and fractionator is provided with the import of rectifying tower refrigerant, rectifying tower tubulation and rectifying tower refrigerant exit; The import of rectifying tower refrigerant and rectifying tower refrigerant exit are all connected with rectifying tower tubulation, and the import of rectifying tower refrigerant is positioned at the below of rectifying tower refrigerant exit.
Described condenser is provided with the import of condenser refrigerant, condenser tubulation and condenser refrigerant exit; The import of condenser refrigerant and condenser refrigerant exit are all connected with condenser tubulation, and the import of condenser refrigerant is positioned at the below of condenser refrigerant exit; Condenser bottom is provided with condenser liquid exit.
Described liquid receiver comprises tank body, and tank body top is provided with liquid receiver liquid-inlet, and tank body bottom is provided with liquid receiver liquid exit, between liquid receiver liquid-inlet and described condenser liquid exit, by pipeline, is connected.
Between the bottom of described rectifying tower and described reaction kettle of the esterification, by two pipelines, be connected, the connectivity part of rectifying tower bottom and two pipelines is respectively rectifying tower gas feed and rectifying tower liquid exit.
Between the bottom of described rectifying tower and described reaction kettle of the esterification, by a pipeline, be connected.
Described final pneumatic outlet comprises condenser pneumatic outlet and liquid receiver pneumatic outlet, and condenser pneumatic outlet is located at the bottom of described condenser, and liquid receiver pneumatic outlet is located at the top of described tank body.
Described final pneumatic outlet is located at arbitrary position on described condenser bottom or described tank body top.
The beneficial effects of the utility model are:
1, on reaction kettle of the esterification still, increased rectifying tower, rectifying tower comprises rectifying column and fractionator, during unsaturated acid gas process fractionator, be condensed, washing unsaturated acid gas refluxes, because the volatility of unsaturated acid and water is different, moisture is concentrated above rectifying column, negative pressure pumping water timesharing, the gas of extracting out significantly reduces containing unsaturated acid, reduced the unsaturated acid consumption in esterifying kettle, even in the situation that lower acid alcohol ratio, esterification time is short, esterification yield is up to 99.5%, and two key retention rates are high.
2, do not use solvent, reduce costs and be conducive to environmental protection, simple and easy to do, without too many complicated installations and facilities.
Accompanying drawing explanation
Fig. 1 is structural representation of the present utility model.
In figure: 1 reaction kettle of the esterification, 2 rectifying tower liquid exits, 3 fillers, 4 rectifying tower refrigerant imports, 5 rectifying tower tubulations, 6 rectifying tower pneumatic outlets, 7 rectifying tower refrigerant exits, 8 rectifying tower gas feeds, 9 tank bodies, 10 condenser liquid exits, 11 condenser tubulations, 12 condenser refrigerant exits, 13 condenser gas feeds, 14 condenser refrigerant imports, 15 condenser pneumatic outlets, 16 liquid receiver liquid-inlets, 17 liquid receiver liquid exits, 18 liquid receiver pneumatic outlets.
Embodiment
Below in conjunction with Figure of description and specific embodiment, the utility model will be further described:
As shown in Figure 1, a kind of polycarboxylate water-reducer rectifying formula esterification system, comprises reaction kettle of the esterification 1, rectifying tower, condenser and liquid receiver; Rectifying tower bottom is connected by pipeline with reaction kettle of the esterification 1, and rectifying tower top is provided with rectifying tower pneumatic outlet 6; Condenser bottom is connected by pipeline with liquid receiver, and condenser top is provided with condenser gas feed 13; Between rectifying tower pneumatic outlet 6 and condenser gas feed 13, by pipeline, be connected, at the terminal portions of system, be also provided with final pneumatic outlet.
Described rectifying tower lower part is rectifying column, and the inside of rectifying column is provided with filler 3, and rectifying tower upper part is fractionator, and fractionator is provided with rectifying tower refrigerant import 4, rectifying tower tubulation 5 and rectifying tower refrigerant exit 7; Rectifying tower refrigerant import 4 and rectifying tower refrigerant exit 7 are all connected with rectifying tower tubulation 5, and rectifying tower refrigerant import 4 is positioned at the below of rectifying tower refrigerant exit 7.
Described condenser is provided with condenser refrigerant import 14, condenser tubulation 11 and condenser refrigerant exit 12; Condenser refrigerant import 14 and condenser refrigerant exit 12 are all connected with condenser tubulation 11, and condenser refrigerant import 14 is positioned at the below of condenser refrigerant exit 12; Condenser bottom is provided with condenser liquid exit 10.
Described liquid receiver comprises tank body 9, and tank body 9 tops are provided with liquid receiver liquid-inlet 16, and tank body 9 bottoms are provided with liquid receiver liquid exit 17, between liquid receiver liquid-inlet 16 and described condenser liquid exit 10, by pipeline, is connected.
Embodiment mono-:
Between the bottom of described rectifying tower and described reaction kettle of the esterification 1, by two pipelines, be connected, the connectivity part of rectifying tower bottom and two pipelines is respectively rectifying tower gas feed 8 and rectifying tower liquid exit 2.Described final pneumatic outlet comprises condenser pneumatic outlet 15 and liquid receiver pneumatic outlet 18, and condenser pneumatic outlet 15 is located at the bottom of described condenser, and liquid receiver pneumatic outlet 18 is located at the top of described tank body 9.
Embodiment bis-:
Between the bottom of described rectifying tower and described reaction kettle of the esterification 1, by a pipeline, be connected.Described final pneumatic outlet comprises condenser pneumatic outlet 15 and liquid receiver pneumatic outlet 18, and condenser pneumatic outlet 15 is located at the bottom of described condenser, and liquid receiver pneumatic outlet 18 is located at the top of described tank body 9.When the bottom of rectifying tower and the pipeline between described reaction kettle of the esterification 1 are when thicker, also two a kind of pipelines of embodiment can be merged into one.
Embodiment tri-:
Between the bottom of described rectifying tower and described reaction kettle of the esterification 1, by two pipelines, be connected, the connectivity part of rectifying tower bottom and two pipelines is respectively rectifying tower gas feed 8 and rectifying tower liquid exit 2.Described final pneumatic outlet is located at arbitrary position on described condenser bottom or described tank body top.When the pipeline that connects when final pneumatic outlet is thicker, condenser pneumatic outlet 15 and liquid receiver pneumatic outlet 18 can be merged into one.
Embodiment tetra-:
Between the bottom of described rectifying tower and described reaction kettle of the esterification 1, by a pipeline, be connected.Described final pneumatic outlet is located at arbitrary position on described condenser bottom or described tank body top.
In above-mentioned whole embodiment, for filler 3, without particular requirement, can, for nonmetal, also can be stainless steel.
Working process of the present utility model is: first rectifying tower refrigerant import 4, rectifying tower refrigerant exit 7, condenser refrigerant import 14, condenser refrigerant exit 12 are all opened, made cold medium flux in suitable scope.At final gas outlet, connect vacuum pump, open vacuum pump, control vacuum tightness in optimum range.
Raw material reacts in reaction kettle of the esterification 1, in reaction process, can produce water, the unsaturated acid gas that water and unsaturated acid mix can enter rectifying tower through piping, unsaturated acid gas is condensed when through rectifying tower, washing unsaturated acid gas refluxes, because the volatility of unsaturated acid and water is different, make moisture above rectifying column and condenser place is concentrated, negative pressure pumping water timesharing, the gas of extracting out significantly reduces containing unsaturated acid, reduced the unsaturated acid consumption in esterifying kettle, even in the situation that lower acid alcohol ratio, esterification time is short, esterification yield is up to 99.5%, two key retention rates are high.
The above, principles more of the present utility model just explain through diagrams, this specification sheets is not in concrete structure and the scope of application described shown in the present invention will being confined to, therefore the corresponding modify being likely utilized every and equivalent, all belong to the scope of the claims that the utility model is applied for.
Except technical characterictic described in specification sheets, all the other technical characterictics are those skilled in the art's known technology.

Claims (8)

1. a polycarboxylate water-reducer rectifying formula esterification system, is characterized in that, comprises reaction kettle of the esterification, rectifying tower, condenser and liquid receiver; Rectifying tower bottom is connected by pipeline with reaction kettle of the esterification, and rectifying tower top is provided with rectifying tower pneumatic outlet; Condenser bottom is connected by pipeline with liquid receiver, and condenser top is provided with condenser gas feed; Between rectifying tower pneumatic outlet and condenser gas feed, by pipeline, be connected, at the terminal portions of system, be also provided with final pneumatic outlet.
2. a kind of polycarboxylate water-reducer rectifying formula esterification system according to claim 1, it is characterized in that, described rectifying tower lower part is rectifying column, the inside of rectifying column is provided with filler, rectifying tower upper part is fractionator, and fractionator is provided with the import of rectifying tower refrigerant, rectifying tower tubulation and rectifying tower refrigerant exit; The import of rectifying tower refrigerant and rectifying tower refrigerant exit are all connected with rectifying tower tubulation, and the import of rectifying tower refrigerant is positioned at the below of rectifying tower refrigerant exit.
3. a kind of polycarboxylate water-reducer rectifying formula esterification system according to claim 2, is characterized in that, described condenser is provided with the import of condenser refrigerant, condenser tubulation and condenser refrigerant exit; The import of condenser refrigerant and condenser refrigerant exit are all connected with condenser tubulation, and the import of condenser refrigerant is positioned at the below of condenser refrigerant exit; Condenser bottom is provided with condenser liquid exit.
4. a kind of polycarboxylate water-reducer rectifying formula esterification system according to claim 3, it is characterized in that, described liquid receiver comprises tank body, tank body top is provided with liquid receiver liquid-inlet, tank body bottom is provided with liquid receiver liquid exit, between liquid receiver liquid-inlet and described condenser liquid exit, by pipeline, is connected.
5. a kind of polycarboxylate water-reducer rectifying formula esterification system according to claim 4, it is characterized in that, between the bottom of described rectifying tower and described reaction kettle of the esterification, by two pipelines, be connected, the connectivity part of rectifying tower bottom and two pipelines is respectively rectifying tower gas feed and rectifying tower liquid exit.
6. a kind of polycarboxylate water-reducer rectifying formula esterification system according to claim 4, is characterized in that, between the bottom of described rectifying tower and described reaction kettle of the esterification, by a pipeline, is connected.
7. according to a kind of polycarboxylate water-reducer rectifying formula esterification system described in claim 5 or 6, it is characterized in that, described final pneumatic outlet comprises condenser pneumatic outlet and liquid receiver pneumatic outlet, condenser pneumatic outlet is located at the bottom of described condenser, and liquid receiver pneumatic outlet is located at the top of described tank body.
8. according to a kind of polycarboxylate water-reducer rectifying formula esterification system described in claim 5 or 6, it is characterized in that, described final pneumatic outlet is located at arbitrary position on described condenser bottom or described tank body top.
CN201320493218.6U 2013-08-13 2013-08-13 Rectification type esterification reaction system for polycarboxylate water reducer Expired - Fee Related CN203474699U (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295022A (en) * 2015-11-13 2016-02-03 鑫统领建材集团有限公司 Method used for preparing polycarboxylate macromonomer
CN116003252A (en) * 2023-02-09 2023-04-25 济南正光化工科技开发有限公司 A kind of preparation method and reaction device of difluoroethyl acetate

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105295022A (en) * 2015-11-13 2016-02-03 鑫统领建材集团有限公司 Method used for preparing polycarboxylate macromonomer
CN116003252A (en) * 2023-02-09 2023-04-25 济南正光化工科技开发有限公司 A kind of preparation method and reaction device of difluoroethyl acetate
CN116003252B (en) * 2023-02-09 2025-03-25 济南正光化工科技开发有限公司 A kind of preparation method and reaction device of difluoroethyl acetate

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Granted publication date: 20140312

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