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Preparation method of 4,4-bis(2-sulfostyryl)-1,1-biphenyl
CN102126991A
China
Worldwide applications
2010
CN
Application CN2010106108613A events
2010-12-29
2011-07-20
Status
Pending
Description
translated from
Technical field
The present invention relates to the chemical additive field, specifically a kind of white dyes 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl.
Background technology
4, two (the 2-sulfonic benzo vinyl)-1 of 4-, 1-biphenyl, a kind of white dyes is called for short CBS-X, has that good anti-chlorine floats, an acid and alkali-resistance, sun-resistant performance, it is the perfect additive of light industry, weaving and daily use chemicals industry, in particular for various washing powder, washing cream, soap, perfumed soap and liquid washing agent, can improve the use properties of product, improve product inner quality and visual appearance.Being specially adapted to cold washing and brightening, is the white dyes kind that is used for the detergent industry best results at present in the world.
The preparation method of CBS-X is in the prior art: in the condensation still, drop into dimethyl formamide (being called for short DMF) earlier, add 4,4 again
,-two and sodium aldehyde (diethoxy phosphonium mesitoyl methyl) biphenyl (abbreviation benzyl ester), ortho-sulfonic acid sodium phenyl aldehyde (being called for short sodium aldehyde), rising temperature for dissolving after insulation half an hour, cools to 45 ℃, when stirring, inwardly drips sodium methoxide solution, continues about 12 hours; After dropwising, be warmed up to 50-55 ℃, continue insulation 3 hours, then cool to below 10 ℃ with cool brine, BS-X crystallizes out with products C; Reaction mass is got to chamber-type press filter with pump carry out solid-liquid separation, filtrate is the mixed solvent of DMF and methyl alcohol, enters rectifying tower again and carries out rectifying, and methyl alcohol is separated with DMF, and residue discards (containing a certain amount of CBS-X product in the residue); The gained filter cake is the CBS-X crude product, crude product is transferred in the refining kettle, add pure water and gac again, be warmed up to 100 ℃ of left and right sides heat filterings, to remove insoluble impurities and gac wherein, filtrate enters into crystallization kettle, cool to below 10 ℃ after adding a certain amount of saturated brine, enter solid-liquid separation, the gained solid is qualified CBS-X product, then dries, packs; Filtrate being contained the saturated brine of few products, carries out sewage disposal.
Above-mentioned preparation process exists following deficiency and defective:
⑴ also contain a spot of CBS-X product owing in the residual solids slag CBS-X product is arranged after having steamed DMF in the saturated brine of refining in addition back, causes the yield of CBS-X to reduce, and ultimate yield has only about 85%;
⑵ refining back saturated brine contains the few products waste residue, promptly contains sodium-chlor and product, if directly deliver to sewage work, and the big cost height of intractability;
⑶ the level of residue of DMF is bigger, is solid waste prods;
⑷ DMF remains in the crude product, has caused the rate of recovery of DMF to reduce, and the DMF rate of recovery is the highest has only 84%, so production cost is higher.
Summary of the invention
The technical problem to be solved in the present invention, provide a kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, this method product yield height, the solid slag generation is little, running cost is low.
For solving the problems of the technologies described above, the technical solution adopted in the present invention is:
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order:
(1) feeds intake-heat up-be incubated
In the condensation still, drop into the solvent dimethyl formamide, be that the ratio of 1:2～2.3 drops into benzyl ester and sodium aldehyde again with the mol ratio, be warming up to 100～120 ℃ of dissolvings, insulation 30～40min cools to 40～45 ℃, inwardly drip sodium methoxide solution while stirring, stir and dropping time remaining 12～13h.
(2) heat up again-insulation again
After dropwising, be warmed up to 50～55 ℃, continue insulation 3～3.5h, to realize the fully purpose of reaction;
(3) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(4) solid-liquid separation
After the condensation still has steamed DMF, inwardly dripping saturated brine (is pure saturated brine for the first time, change the saturated brine that contains product after making with extra care later on into), the CBS-X product of generation is dissolved in the water, be cooled to 8～15 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(51) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(52) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds ℃ filtration of gac heat to 100 with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 8～15 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used next preparation round-robin solid-liquid separation step.
Provided by the present invention 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the above-mentioned preparation method of 1-biphenyl, step (1)～(2) are same as the prior art, and it is the different of subsequent step with the difference of prior art, and the present invention has following characteristics:
Production process does not produce the DMF waste residue, and level of residue has also reduced by 80% in the water, therefore greatly reduces the generation of solid slag.
In the solid-liquid separation of after condensation reaction, carrying out, there are the methyl alcohol of flavor and DMF to be distilled out in advance owing to inflammable, and are stored in the storage tank of sealing, thereby reduced security risk.
To sum up, the present invention compared with prior art, obtained technical progress is: this method product yield height, the solid slag generation is little, running cost is low, security risk reduces.The present invention can be used for preparing 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, and 1-biphenyl is for various washing powder, washing cream, soap, perfumed soap and liquid washing agent provide white dyes.
The present invention is described in further detail below in conjunction with specific embodiment.
Embodiment
Following examples only are used to the present invention that remarks additionally, and are not qualification of the present invention.
Embodiment 1-5 is preparation 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, and the method for 1-biphenyl is utilized benzyl ester and sodium aldehyde to carry out condensation reaction and is made.Embodiment 1-5 carries out successively.
Embodiment 1
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order: (11) feed intake-heat up-be incubated
In 3000L condensation still, drop into 1200kg dimethyl formamide (being called for short DMF) earlier, add the benzyl ester of 1kmol and the sodium aldehyde of 2kmol again, be warming up to 100 ℃ of dissolvings, insulation 40min cools to 42 ℃; When stirring, inwardly drip sodium methoxide solution 450L, drip time remaining 12.5h;
(12) heat up again-insulation again
After dropwising, be warmed up to 50 ℃, continue insulation 3.2h;
(13) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(14) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip saturated brine, the CBS-X product of generation is dissolved in the water, be cooled to 12 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(151) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(152) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac in 100 ℃ of heat filterings with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 12 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used (24) solid-liquid separation step (being that the waste water that this operation produces is applied mechanically) among the embodiment 2.
Embodiment 2
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order: (21) feed intake-heat up-be incubated
In 3000L condensation still, drop into 1200kg dimethyl formamide (being called for short DMF) earlier, add 1kmol benzyl ester and 2.1kmol sodium aldehyde again, be warming up to 120 ℃ of dissolvings, insulation 35min cools to 45 ℃; When stirring, inwardly drip sodium methoxide solution 450L, drip time remaining 12h;
(22) heat up again-insulation again
After dropwising, be warmed up to 52 ℃, continue insulation 3.5h;
(23) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(24) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip the saturated brine that step among the embodiment 1 (152) gained contains product, the CBS-X product of generation is dissolved in the water, be cooled to 15 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(251) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(252) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac in 100 ℃ of heat filterings with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 8 ℃ and carries out crystallization, and carry out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used (34) solid-liquid separation step (being that the waste water that this operation produces is applied mechanically) among the embodiment 3.
Embodiment 3
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order: (31) feed intake-heat up-be incubated
In 3000L condensation still, drop into 1200kg dimethyl formamide (being called for short DMF) earlier, add 1kmol benzyl ester and 2.25kmol sodium aldehyde again, be warming up to 105 ℃ of dissolvings, insulation 38min cools to 41 ℃; When stirring, inwardly drip sodium methoxide solution 450L, drip time remaining 12.2h;
(32) heat up again-insulation again
After dropwising, be warmed up to 53 ℃, continue insulation 3.1h;
(33) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(34) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip the saturated brine that step among the embodiment 2 (252) gained contains product, the CBS-X product of generation is dissolved in the water, be cooled to 13 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(351) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(352) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac in 100 ℃ of heat filterings with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 11 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used (44) solid-liquid separation step (being that the waste water that this operation produces is applied mechanically) among the embodiment 4.
Embodiment 4
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order:
(41) feed intake-heat up-be incubated
In 3000L condensation still, drop into 1200kg dimethyl formamide (being called for short DMF) earlier, add 1kmol benzyl ester and 2.28kmol sodium aldehyde again, be warming up to 110 ℃ of dissolvings, insulation 30min cools to 43 ℃; When stirring, inwardly drip sodium methoxide solution 450L, drip time remaining 12.6h;
(42) heat up again-insulation again
After dropwising, be warmed up to 54 ℃, continue insulation 3.3h;
(43) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(44) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip the saturated brine that step among the embodiment 3 (352) gained contains product, the CBS-X product of generation is dissolved in the water, be cooled to 10 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(451) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(452) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac in 100 ℃ of heat filterings with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 13 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used (54) solid-liquid separation step (being that the waste water that this operation produces is applied mechanically) among the embodiment 5.
Embodiment 5
A kind of 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl, carry out according to the following steps order: (51) feed intake-heat up-be incubated
In 3000L condensation still, drop into 1200kg dimethyl formamide (being called for short DMF) earlier, add 1kmol benzyl ester and 2.3kmol sodium aldehyde again, be warming up to 115 ℃ of dissolvings, insulation 33min cools to 40 ℃; When stirring, inwardly drip sodium methoxide solution 450L, drip time remaining 12.8h;
(52) heat up again-insulation again
After dropwising, be warmed up to 53 ℃, continue insulation 3.1h;
(53) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(54) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip the saturated brine that step among the embodiment 4 (452) gained contains product, the CBS-X product of generation is dissolved in the water, be cooled to 8 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(551) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(552) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac in 100 ℃ of heat filterings with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 10 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used the solid-liquid separation step (being that the waste water that this operation produces is applied mechanically) in next preparation circulation.
Claims (1)
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Claims (1)
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1. one kind 4, two (the 2-sulfonic benzo vinyl)-1 of 4-, the preparation method of 1-biphenyl is characterized in that: this method is carried out according to the following steps order:
(1) feeds intake-heat up-be incubated
In the condensation still, drop into the solvent dimethyl formamide, be that the ratio of 1:2 drops into benzyl ester and sodium aldehyde again with the mol ratio, be warming up to 100～120 ℃ of dissolvings, insulation 30～40min cools to 40～45 ℃, inwardly drip sodium methoxide solution while stirring, stir and dropping time remaining 12～13h;
(2) heat up again-insulation again
After dropwising, be warmed up to 50～55 ℃, continue insulation 3～3.5h;
(3) continue intensification-distillation-rectifying separation
Continue to heat up, directly the methyl alcohol in the reaction system and DMF are steamed and enter rectifying tower and separate;
(4) solid-liquid separation
After the condensation still has steamed DMF, inwardly drip saturated brine, the CBS-X product of generation is dissolved in the water, be cooled to 8～15 ℃ again and carry out solid-liquid separation, get saturated brine and CBS-X crude product, handle respectively;
(51) saturated brine is handled
Solid-liquid separation gained saturated brine directly enters into evaporating kettle, distills, and steam is used for other place with cold water condensation gained water of condensation, Gu the useless conventional processing of carrying out;
(52) CBS-X crude product refining
Solid-liquid separation gained CBS-X crude product adds gac heat 100 ℃ of filtrations with water of condensation dilution dissolving, and filtrate enters into crystallization kettle, adds saturated brine, is cooled to 8～15 ℃ of crystallizations, and carries out solid-liquid separation, and the gained solid is qualified CBS-X product; Filtrate being contained the saturated brine of few products, and cover is used next preparation round-robin solid-liquid separation step.