CN102795963A - Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method - Google Patents
Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method Download PDFInfo
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- CN102795963A CN102795963A CN2012103355849A CN201210335584A CN102795963A CN 102795963 A CN102795963 A CN 102795963A CN 2012103355849 A CN2012103355849 A CN 2012103355849A CN 201210335584 A CN201210335584 A CN 201210335584A CN 102795963 A CN102795963 A CN 102795963A
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Abstract
The invention discloses a process for preparing trimethylolpropane by adopting a centrifugal filtering calcium method. The preparation process is characterized by comprising the following steps of: condensing and performing a formic acid neutralization reaction by taking n-butyl aldehyde and formaldehyde as raw materials and taking technical grade calcium hydroxide as a basic catalyst to obtain a crude trimethylolpropane reaction liquid which contains di-trimethylolpropane and calcium formate serving as side products; and separating solid phase residues from the reaction liquid in a horizontal spiral centrifugal filtering way, concentrating, recovering, refining trimethylolpropane and tableting. Compared with a plate type filter press separating method, the process has the advantage: a settling process before separating and an extracting process after separating are reduced. The arrangement of a settling tank is saved, the floor area of the entire process is reduced, and over two hours of settling time is saved; the generation of a large amount of washing sewage in a production process is avoided; and due to the reduction in extraction, the consumption of an extracting agent is saved, and the production efficiency is increased.
Description
Technical field
The invention belongs to chemical technology field; Relate to a kind of employing centrifuging formula calcium method TriMethylolPropane(TMP) preparation technology, be specifically related to the novel process that a kind of centrifuging mode that in the filtration operation of calcium method TriMethylolPropane(TMP) reaction solution, adopts horizontal screw unloading replaces the board-like press filtration mode of primary.
Background technology
In industry, TMP mainly is to be main raw material with butyraldehyde-n and formaldehyde, and condensation reaction makes midbody dihydroxymethyl butyraldehyde under the basic catalyst effect, and this midbody further generates TriMethylolPropane(TMP) with formolite reaction.
The production technique of at present domestic TriMethylolPropane(TMP) is divided into two kinds of sodium method and calcium methods, and promptly raw material uses sodium hydroxide or calcium hydroxide respectively.Calcium method technology is because of having that flow process is short, cost is low, labour intensity is low and advantage such as environmental protection and energy saving, replacement sodium method technology gradually.But in the reaction process when production process, because of containing impurity such as Marinco H, ironic hydroxide, white lake in the calcium hydroxide, these impurity all existed with the form of suspended substance after reaction was accomplished, and filtered operation so must behind reaction process, add.Existing filtration operation all adopts plate type pressure filter, and reaction solution is carried out standing sedimentation, and five subsiders are set, and each settling time, after the sedimentation, upper strata liquid filtered with plate type pressure filter, also need pass through extraction process after the filtering separation more than 2 hours.A large amount of about 6-10m of wash water can appear in the production process
3/ h, and need occupy very big area, need very big manpower to carry out the scarfing cinder desilting, need frequent replacing filter cloth.Therefore traditional filtration process has not only been wasted lot of manpower and material resources, and the large amount of sewage that produces has also caused certain harm to environment.
Summary of the invention
The object of the invention just is to provide a kind of employing centrifuging formula calcium method TriMethylolPropane(TMP) preparation technology.Board-like relatively press filtration separation method, settling process before omission separates and the extraction process after the separation.
Technical solution of the present invention: with butyraldehyde-n and formaldehyde is raw material; Use technical grade calcium hydroxide to be basic catalyst; Through condensation and formic acid neutralization reaction, obtain containing the TriMethylolPropane(TMP) bullion reaction solution that comprises ditrimethylolpropane and calcium formiate sub product; Adopt horizontal spiral centrifuging mode that reaction solution is carried out the separation of solid phase residue, settling process before omission separates in the whole technology and the extraction process after the separation.
Preferred its preparation technology is following:
(1) condensation and neutralization: in the reaction kettle of whisking appliance is housed; Adding mol ratio is butyraldehyde-n and the formaldehyde raw material of 1:3, is basic catalyst with technical grade calcium hydroxide, and stirring is warmed up to 50-70 ℃ and carries out condensation reaction; Obtain 2 in the reaction process; 2-dihydroxymethyl butyraldehyde, formaldehyde carries out Cannizzaro reaction again, and every mole of above-mentioned butyraldehyde-n adds 0.2-0.4 mole formaldehyde again; Then in reaction kettle, add formic acid and neutralize and reach pH value 5-7, promptly obtain containing the TriMethylolPropane(TMP) bullion reaction solution that comprises ditrimethylolpropane and calcium formiate sub product;
(2) centrifuging: through the TriMethylolPropane(TMP) bullion reaction solution of transferpump with step (1); Squeeze in the rotary drum of horizontal spiral centrifuge; The powerful cf-of rotary drum generation through high speed rotating is deposited to drum inner wall to the big solid phase particles of density, because the rotating speed of spiral and rotary drum is different, the two has relative movement; Utilize the relative movement of spiral and rotary drum to push the solid phase that is deposited on drum inner wall the discharge of to rotary drum exit, the clear liquid after the separation is discharged from the whizzer the other end; Thereby accomplished the separation of solid phase residue in the TriMethylolPropane(TMP) bullion reaction solution;
Solid phase residue staple is: white lake, Marinco H, quicklime etc.
(3) concentrate recovery: the reaction solution after step (2) is obtained separating is sent into upgrading tower and is concentrated, and reclaims unreacted formaldehyde through the distillation of double tower cat head; Recovery formaldehyde returns in the step (1) and recycles, simultaneously, and the small amount of methanol sub product that the recovered overhead side reaction obtains; Be TriMethylolPropane(TMP) and calcium formiate liquid concentrator at the bottom of the tower, column bottom temperature is controlled to be 120-135 when spending, and the recovery calcium formiate is separated out in the calcium formiate crystallization;
(4) TriMethylolPropane(TMP) rectifying: will pass through the liquid concentrator that step (3) obtains and then carry out rectifying, control separates different cuts can obtain TriMethylolPropane(TMP);
(5) TriMethylolPropane(TMP) film-making:, directly send into pelleter cooling and slice packaging through the smart TriMethylolPropane(TMP) product of rectifying.
The rotating speed of horizontal spiral centrifuge high speed rotating is more than the 3000 commentaries on classics/min, and the filter pore of the built-in filtering net of horizontal spiral centrifuge is 500-1000 orders.
Earlier in TriMethylolPropane(TMP) bullion reaction solution, adds flocculation agent in the step (2), the volume ratio of flocculation agent and TriMethylolPropane(TMP) bullion reaction solution is 1:580-650, leave standstill 5-8 minutes after, squeeze into again in the rotary drum of horizontal spiral centrifuge.
Said flocculation agent is a SEPIGEL 305, and the volume ratio of SEPIGEL 305 and TriMethylolPropane(TMP) bullion reaction solution is 1:600.
Beneficial effect of the present invention:
1. the separation efficiency of horizontal spiral centrifuge is high, floor space is little, and the rotating speed of high speed rotating reaches more than 3000, thereby solid-liquid is separated mutually more easily, and LW-450 a type horizontal screw unloading whizzer can replace 4 40m of traditional technology
2Plate type pressure filter.
2. do not have waste water in the production process, can not work the mischief to environment because of waste water.
3. the solid phase sediment is successional in the production process goes out to the slag car, has saved lot of manpower and material resources.
4. horizontal spiral centrifuge can turn round by successive automatically, and is easy to maintenance.
5. board-like relatively press filtration separation method, the present invention reduces the extraction process after preceding settling process of separation and the separation.Save the setting of subsider, reduced the floor space of whole technology, saved the settling time more than 2 hours; Stopped the generation of a large amount of wash waters in the production process; The minimizing of extraction, the consumption of having practiced thrift extraction agent has improved production efficiency.
6. in sum, but technology operate continuously of the present invention is suitable for suitability for industrialized production.
Description of drawings
Fig. 1 is the process flow sheet of the embodiment of the invention 1.
Fig. 2 is the structural representation of the LW horizontal spiral centrifuge of the embodiment of the invention 1.
Among Fig. 1: reaction liquid bath 1, extraction pump 2, horizontal spiral centrifuge 3, the slag car 4, stillness of night groove 5, extraction pump 6, feed-pipe 7, support 8, casing 9, defeated material spiral 10, rotary drum 11, chock 12, differential mechanism 13, pulley 14 sinks and mixes 15, clear liquor 16.
Embodiment
The present invention can do further description to the present invention through following embodiment, yet scope of the present invention is not limited to following embodiment.
Embodiment 1:
(1) feed intake according to the 10mol butyraldehyde-n, formaldehyde, butyraldehyde-n, calcium hydroxide feed intake according to 3.2:1:0.8, and the mass content of calcium hydroxide is 90%, obtain reaction solution and separate, and start screw centrifuge with rotating speed 3000 commentaries on classics/min.Centrifugally come out to be limpid mother liquor; Removal of impurity 98%; Concrete operations are: the reaction solution extraction pump 2 in the reaction liquid bath 1 that contains suspended solid among Fig. 1 is adopted to horizontal spiral centrifuge 3, gets in the rotary drum 11 through feed-pipe 7, and the powerful cf-that the rotary drum 11 of high speed rotating produces makes solid phase be deposited to the inwall net 12 of rotary drum; Defeated material spiral 10 is because of different generation relative movement with the rotating speed of rotary drum 11; Solid phase is flowed out in the slag cars 4 from heavy assorted 15, and liquid phase then flow in the stillness of night groove 5 from clear liquor 16, the solution in the clear liquid groove 5 through another extraction pump 6 extraction to subsequent handling.
(2) centrifugal mother liquor entering upgrading tower evaporates, and in concentration process, isolates calcium formiate, three hydroxyl solution is carried out the light constituent knockout tower carry out rectifying, carries out the distillation of three hydroxyl knockout towers at last and obtains TriMethylolPropane(TMP).Obtain TriMethylolPropane(TMP) 2.08kg.
CH
3CH
2CH
2CH0+HCHO → CH
3CH
3C (CH2OH)
310 moles butyraldehyde-n reaction generates 10 moles TriMethylolPropane(TMP).134.18 * 10/72.12=2495.28g TriMethylolPropane(TMP) in theory.Experiment obtains the 2.08kg TriMethylolPropane(TMP).Yield is 2080/2495.28=83.3%.
Embodiment 2:
(1) feed intake according to the 10mol butyraldehyde-n, formaldehyde, butyraldehyde-n, calcium hydroxide feed intake according to 3.2:1:0.8, and (calcium hydroxide content 90%) obtains reaction solution and separates, and start screw centrifuge with rotating speed 3500 commentaries on classics/min.Centrifugally come out to be limpid mother liquor, removal of impurity 99%, concrete operations are identical with embodiment 1;
(2) centrifugal mother liquor entering upgrading tower evaporates, and in concentration process, isolates calcium formiate, three hydroxyl solution is carried out the light constituent knockout tower carry out rectifying, carries out the distillation of three hydroxyl knockout towers at last and obtains three hydroxyls.Obtaining mass content is 99.5% TriMethylolPropane(TMP) 2.101kg, is 84.2% with the butyraldehyde-n rate of collecting.
Embodiment 3:
(1) feed intake according to the 10mol butyraldehyde-n, formaldehyde, butyraldehyde-n, calcium hydroxide feed intake according to 3.2:1:0.8, and (calcium hydroxide content 90%) obtains reaction solution and separates, and start screw centrifuge with rotating speed 4000 commentaries on classics/min.Centrifugally come out to be limpid mother liquor, removal of impurity 99%, concrete operations are identical with embodiment 1;
(2) centrifugal mother liquor entering upgrading tower evaporates, and in concentration process, isolates calcium formiate, three hydroxyl solution is carried out the light constituent knockout tower carry out rectifying, carries out the distillation of three hydroxyl knockout towers at last and obtains TriMethylolPropane(TMP).Obtaining mass content is 99.5% TriMethylolPropane(TMP) 2.053kg, is 82.2% with the butyraldehyde-n rate of collecting.
Board-like relatively press filtration separation method among the embodiment 1-3 omits the settling process before separating, and has saved the settling time more than 2 hours, has saved the setting of subsider, has reduced the floor space of about 6 square meters; Separate the back and omit extraction process, the generation of 0.08 side's wash water in the production process has been stopped in the consumption of having practiced thrift the 0.02-0.03kg extraction agent.
Adopt the inventive method, produce 10000 tons of TriMethylolPropane(TMP)s per year, board-like relatively press filtration separation method; Omit the settling process before separating; Saved the settling time more than 2 hours for single batch, saved the setting of subsider, reduced by about 80 square metres floor space; Separate the back and omit extraction process, the generation of about 30,000 side's wash waters in the production process has been stopped in the consumption of having practiced thrift 200-300 tons of extraction agents, has improved production efficiency widely.
Among the embodiment 1-3, can in TriMethylolPropane(TMP) bullion reaction solution, add the flocculation agent SEPIGEL 305 earlier, the volume ratio of SEPIGEL 305 and TriMethylolPropane(TMP) bullion reaction solution is 1:580-650, and is preferred: 1:600; After leaving standstill 5-8 minutes, squeeze into again in the rotary drum of horizontal spiral centrifuge.
Claims (4)
1. one kind is adopted centrifuging formula calcium method TriMethylolPropane(TMP) preparation technology, is raw material with butyraldehyde-n and formaldehyde, uses technical grade calcium hydroxide to be basic catalyst, it is characterized in that its preparation technology is following:
(1) condensation and neutralization: in the reaction kettle of whisking appliance is housed; Adding mol ratio is butyraldehyde-n and the formaldehyde raw material of 1:3, is basic catalyst with technical grade calcium hydroxide, and stirring is warmed up to 50-70 ℃ and carries out condensation reaction; Obtain 2 in the reaction process; 2-dihydroxymethyl butyraldehyde, formaldehyde carries out Cannizzaro reaction again, and every mole of above-mentioned butyraldehyde-n adds 0.2-0.4 mole formaldehyde again; Then in reaction kettle, add formic acid and neutralize and reach pH value 5-7, promptly obtain containing the TriMethylolPropane(TMP) bullion reaction solution that comprises ditrimethylolpropane and calcium formiate sub product;
(2) centrifuging: through the TriMethylolPropane(TMP) bullion reaction solution of transferpump with step (1); Squeeze in the rotary drum of horizontal spiral centrifuge; The powerful cf-of rotary drum generation through high speed rotating is deposited to drum inner wall to the big solid phase particles of density, because the rotating speed of spiral and rotary drum is different, the two has relative movement; Utilize the relative movement of spiral and rotary drum to push the solid phase that is deposited on drum inner wall the discharge of to rotary drum exit, the clear liquid after the separation is discharged from the whizzer the other end; Thereby accomplished the separation of solid phase residue in the TriMethylolPropane(TMP) bullion reaction solution;
(3) concentrate recovery: the reaction solution after step (2) is obtained separating is sent into upgrading tower and is concentrated, and reclaims unreacted formaldehyde through the distillation of double tower cat head; Recovery formaldehyde returns in the step (1) and recycles, simultaneously, and the small amount of methanol sub product that the recovered overhead side reaction obtains; Be TriMethylolPropane(TMP) and calcium formiate liquid concentrator at the bottom of the tower, column bottom temperature is controlled to be 120-135 when spending, and the recovery calcium formiate is separated out in the calcium formiate crystallization;
(4) TriMethylolPropane(TMP) rectifying: will pass through the liquid concentrator that step (3) obtains and then carry out rectifying, control separates different cuts can obtain TriMethylolPropane(TMP);
(5) TriMethylolPropane(TMP) film-making:, directly send into pelleter cooling and slice packaging through the smart TriMethylolPropane(TMP) product of rectifying.
2. preparation technology as claimed in claim 1 is characterized in that: the rotating speed of horizontal spiral centrifuge high speed rotating is more than the 3000 commentaries on classics/min, and the filter pore of the built-in filtering net of horizontal spiral centrifuge is 500-1000 orders.
3. according to claim 1 or claim 2 preparation technology; It is characterized in that: in TriMethylolPropane(TMP) bullion reaction solution, add flocculation agent earlier in the step (2); The volume ratio of flocculation agent and TriMethylolPropane(TMP) bullion reaction solution is 1:580-650; After leaving standstill 5-8 minutes, squeeze into again in the rotary drum of horizontal spiral centrifuge.
4. preparation technology as claimed in claim 3 is characterized in that: said flocculation agent is a SEPIGEL 305, and the volume ratio of SEPIGEL 305 and TriMethylolPropane(TMP) bullion reaction solution is 1:600.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369332A (en) * | 2018-11-27 | 2019-02-22 | 濮阳市永安化工有限公司 | The processing method of calcium ash in calcium method trimethylolpropane preparation process |
| CN110357761A (en) * | 2019-07-25 | 2019-10-22 | 江西科顶化学材料有限公司 | A kind of production technology of trimethylolethane |
| CN114031481A (en) * | 2021-11-24 | 2022-02-11 | 赤峰瑞阳化工有限公司 | Extraction and calcium removal method for trimethylolpropane production |
| CN115536491A (en) * | 2021-09-30 | 2022-12-30 | 湖北宜化化工科技研发有限公司 | Production method for producing trimethylolpropane by recycling carbide slag |
| CN115745742A (en) * | 2022-12-16 | 2023-03-07 | 赤峰瑞阳化工有限公司 | Method for recycling residual aldehyde from calcium-method trimethylolpropane condensation liquid |
| CN117263780A (en) * | 2023-09-18 | 2023-12-22 | 深圳市普利凯新材料股份有限公司 | Preparation method of trimethylolpropane diallyl ether |
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| US7253326B1 (en) * | 2006-03-07 | 2007-08-07 | Lg Chem, Ltd. | Method for preparing trimethylolproane |
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| CN1428323A (en) * | 2001-12-27 | 2003-07-09 | 拜尔公司 | Process for preparing trialkyl methylpropane |
| US7253326B1 (en) * | 2006-03-07 | 2007-08-07 | Lg Chem, Ltd. | Method for preparing trimethylolproane |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109369332A (en) * | 2018-11-27 | 2019-02-22 | 濮阳市永安化工有限公司 | The processing method of calcium ash in calcium method trimethylolpropane preparation process |
| CN110357761A (en) * | 2019-07-25 | 2019-10-22 | 江西科顶化学材料有限公司 | A kind of production technology of trimethylolethane |
| CN115536491A (en) * | 2021-09-30 | 2022-12-30 | 湖北宜化化工科技研发有限公司 | Production method for producing trimethylolpropane by recycling carbide slag |
| CN115536491B (en) * | 2021-09-30 | 2024-04-12 | 湖北宜化化工科技研发有限公司 | Production method for producing trimethylolpropane by recycling carbide slag |
| CN114031481A (en) * | 2021-11-24 | 2022-02-11 | 赤峰瑞阳化工有限公司 | Extraction and calcium removal method for trimethylolpropane production |
| CN115745742A (en) * | 2022-12-16 | 2023-03-07 | 赤峰瑞阳化工有限公司 | Method for recycling residual aldehyde from calcium-method trimethylolpropane condensation liquid |
| CN117263780A (en) * | 2023-09-18 | 2023-12-22 | 深圳市普利凯新材料股份有限公司 | Preparation method of trimethylolpropane diallyl ether |
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Denomination of invention: Process for preparing trimethylolpropane by adopting centrifugal filtering calcium method Effective date of registration: 20191226 Granted publication date: 20130710 Pledgee: Dongxiang sub branch of Jiujiang Bank Co.,Ltd. Pledgor: JIANGXI KOSIN ORGANIC CHEMICAL Co.,Ltd. Registration number: Y2019360000049 |
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Address after: 331800 yuanshangang Industrial Park, Dongxiang Economic Development Zone, Dongxiang District, Fuzhou City, Jiangxi Province Patentee after: Jiangxi Gaoxin Frontier Technology Co.,Ltd. Address before: No.1 yuanshangang, Dongxiang County, Fuzhou City, Jiangxi Province Patentee before: JIANGXI KOSIN ORGANIC CHEMICAL Co.,Ltd. |
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Date of cancellation: 20230206 Granted publication date: 20130710 Pledgee: Dongxiang sub branch of Jiujiang Bank Co.,Ltd. Pledgor: JIANGXI KOSIN ORGANIC CHEMICAL Co.,Ltd. Registration number: Y2019360000049 |