CN102977628A - One-pot synthesis method of fluorescent brightener ER-II - Google Patents
One-pot synthesis method of fluorescent brightener ER-II Download PDFInfo
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- CN102977628A CN102977628A CN2012105557563A CN201210555756A CN102977628A CN 102977628 A CN102977628 A CN 102977628A CN 2012105557563 A CN2012105557563 A CN 2012105557563A CN 201210555756 A CN201210555756 A CN 201210555756A CN 102977628 A CN102977628 A CN 102977628A
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Abstract
The invention belongs to the technical field of synthesis of fluorescent brightener ER-II, and particularly relates to a one-pot synthesis method of fluorescent brightener ER-II. The one-pot synthesis method comprises the following steps: adding 390-410 kg of diethyl o-cyanobenzyl phosphonate into a reaction kettle, stirring for 5 minutes, and then stopping stirring; adding 205-215 kg of p-phthalaldehyde, and stirring again; adding assistant, and thoroughly stirring; adding 345-355 kg of diethyl p-cyanobenzyl phosphonate, and stirring until the temperature is cooled to 20 DEG C; starting to dropwisely add 290 kg of 28% (mass percent) sodium methoxide solution, wherein the addition of the sodium methoxide solution needs to be finished in 5 hours; after the addition is finished, keeping the temperature for 3 hours, and moving out of the reaction kettle; and when the temperature is cooled to 15 DEG C, centrifuging, boiling in water, and drying to obtain the finished product.
Description
Technical field
The invention belongs to the synthetic technical field of fluorescent whitening agent ER-II type, be specifically related to the one-pot synthesis of fluorescent whitening agent ER-II type.
Background technology
Traditional synthetic fluorescent whitening agent ER-II type divides two step method synthetic, be respectively a step condensation and two step condensations, adopt two pots of synthesis methods of fluorescent whitening agent ER-II type, dividing two pots carries out, its raw material availability is low, only has about 76% for the utilization ratio of terephthalaldehyde, and complicated operation, energy consumption is high, and cost is high.
Summary of the invention
The object of the invention is to for the defective of above-mentioned existence and the one-pot synthesis of fluorescent whitening agent ER-II type be provided,
Technical scheme of the present invention is: the one-pot synthesis of fluorescent whitening agent ER-II type, its step is as follows: with 390-410kg
The o-cyanobenzyl diethyl phosphoric acid is added in the reactor, during question response still temperature to 40 ℃, the dimethyl formamide (DMF) that adds 950-1050kg, stir after 5 minutes, stop to stir, add the 205-215kg terephthalaldehyde, re-start stirring, during question response still temperature to 5 ℃, begin to drip massfraction and be 28% sodium methoxide solution 580-600kg, drip off sodium methoxide solution with 5～6 hours, be added dropwise to complete rear insulation 3 hours, after the adding auxiliary agent fully stirs, add 345-355kg to cyano group benzyl diethyl phosphoric acid, when temperature of reaction kettle is 50 ℃, add 300kg dimethyl formamide (DMF), be stirred to temperature and be down to 20 ℃, begin to drip massfraction and be 28% sodium methoxide solution 290kg, drip off sodium methoxide solution with 5 hours, be added dropwise to complete rear insulation 3 hours, produce reactor and treat that temperature is down to 15 ℃, through centrifugal, poach, oven dry obtains finished product.
Described auxiliary agent is Glacial acetic acid.
Beneficial effect of the present invention is: adopt the one-pot synthesis of fluorescent whitening agent ER-II type, saved middle sepn process, after insulation is finished in a contracting, add auxiliary agent, undertaken by two contracting steps after fully stirring.Finish in one pot, its raw material availability can improve, and the utilization ratio of terephthalaldehyde is more than 80%, and simple to operate, and energy consumption, cost are relatively low, have reduced simultaneously employee's labour intensity, have reduced environmental pollution factors.
Embodiment
The one-pot synthesis of fluorescent whitening agent ER-II type, its step is as follows: 400kg o-cyanobenzyl diethyl phosphoric acid is added in the reactor, during question response still temperature to 40 ℃, the dimethyl formamide (DMF) that adds 700kg, stir after 5 minutes, stop to stir, add the 210kg terephthalaldehyde, re-start stirring, during question response still temperature to 5 ℃, begin to drip massfraction and be 28% sodium methoxide solution 590kg, with dripping off sodium methoxide solution in 5～6 hours, be added dropwise to complete rear insulation 3 hours, add after Glacial acetic acid 10kg fully stirs, add 350kg to cyano group benzyl diethyl phosphoric acid, when being 50 ℃, temperature of reaction kettle adds 300kg dimethyl formamide (DMF), be stirred to temperature and be down to 20 ℃, begin to drip massfraction and be 28% sodium methoxide solution 290kg, with dripping off sodium methoxide solution in 5 hours, be added dropwise to complete rear insulation 3 hours, produce reactor and treat that temperature is down to 15 ℃, through centrifugal, poach, oven dry obtains finished product.
Claims (2)
1. the one-pot synthesis of fluorescent whitening agent ER-II type, its step is as follows: 390-410kg o-cyanobenzyl diethyl phosphoric acid is added in the reactor, during question response still temperature to 40 ℃, the dimethyl formamide (DMF) that adds 950-1050kg, stir after 5 minutes, stop to stir, add the 205-215kg terephthalaldehyde, re-start stirring, during question response still temperature to 5 ℃, begin to drip massfraction and be 28% sodium methoxide solution 580-600kg, with dripping off sodium methoxide solution in 5～6 hours, be added dropwise to complete rear insulation 3 hours, add after auxiliary agent fully stirs, add 345-355kg to cyano group benzyl diethyl phosphoric acid, when being 50 ℃, temperature of reaction kettle adds 300kg dimethyl formamide (DMF), be stirred to temperature and be down to 20 ℃, begin to drip massfraction and be 28% sodium methoxide solution 290kg, with dripping off sodium methoxide solution in 5 hours, be added dropwise to complete rear insulation 3 hours, produce reactor and treat that temperature is down to 15 ℃, through centrifugal, poach, oven dry obtains finished product.
2. the one-pot synthesis of fluorescent whitening agent ER according to claim 1-II type is characterized in that, described auxiliary agent is Glacial acetic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012105557563A CN102977628A (en) | 2012-12-20 | 2012-12-20 | One-pot synthesis method of fluorescent brightener ER-II |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012105557563A CN102977628A (en) | 2012-12-20 | 2012-12-20 | One-pot synthesis method of fluorescent brightener ER-II |
Publications (1)
| Publication Number | Publication Date |
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| CN102977628A true CN102977628A (en) | 2013-03-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2012105557563A Pending CN102977628A (en) | 2012-12-20 | 2012-12-20 | One-pot synthesis method of fluorescent brightener ER-II |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4380514A (en) * | 1980-01-12 | 1983-04-19 | Basf Aktiengesellschaft | Preparation of optical brighteners |
| CN1817857A (en) * | 2006-03-21 | 2006-08-16 | 华东理工大学 | Production of 1,4-bis(O-styryl) |
| WO2007023087A1 (en) * | 2005-08-23 | 2007-03-01 | Basf Aktiengesellschaft | Liquid detergent formulation |
| EP1725708B1 (en) * | 2004-03-11 | 2007-07-18 | Basf Aktiengesellschaft | Method for optical brightening of synthetic fibres or of synthetic fibres mixed with natural fibres |
| JP2008530324A (en) * | 2005-02-17 | 2008-08-07 | アルケマ フランス | Molded article showing multicolor effect, and associated optical device and resin |
| CN101357897A (en) * | 2008-09-05 | 2009-02-04 | 浙江传化华洋化工有限公司 | Method for preparing dicyano-1,4phenylethenes asymmetric fluorescent whitener |
| WO2012098015A1 (en) * | 2011-01-20 | 2012-07-26 | Huntsman Advanced Materials (Switzerland) Gmbh | Formulations of fluorescent whitening agents in dispersed form |
-
2012
- 2012-12-20 CN CN2012105557563A patent/CN102977628A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4380514A (en) * | 1980-01-12 | 1983-04-19 | Basf Aktiengesellschaft | Preparation of optical brighteners |
| EP1725708B1 (en) * | 2004-03-11 | 2007-07-18 | Basf Aktiengesellschaft | Method for optical brightening of synthetic fibres or of synthetic fibres mixed with natural fibres |
| JP2008530324A (en) * | 2005-02-17 | 2008-08-07 | アルケマ フランス | Molded article showing multicolor effect, and associated optical device and resin |
| WO2007023087A1 (en) * | 2005-08-23 | 2007-03-01 | Basf Aktiengesellschaft | Liquid detergent formulation |
| CN1817857A (en) * | 2006-03-21 | 2006-08-16 | 华东理工大学 | Production of 1,4-bis(O-styryl) |
| CN101357897A (en) * | 2008-09-05 | 2009-02-04 | 浙江传化华洋化工有限公司 | Method for preparing dicyano-1,4phenylethenes asymmetric fluorescent whitener |
| WO2012098015A1 (en) * | 2011-01-20 | 2012-07-26 | Huntsman Advanced Materials (Switzerland) Gmbh | Formulations of fluorescent whitening agents in dispersed form |
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Application publication date: 20130320 |