CN1124248C - Process for preparing muskxylol by chemical reaction on waste musk ketone dregs - Google Patents
Process for preparing muskxylol by chemical reaction on waste musk ketone dregs Download PDFInfo
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- CN1124248C CN1124248C CN 01100572 CN01100572A CN1124248C CN 1124248 C CN1124248 C CN 1124248C CN 01100572 CN01100572 CN 01100572 CN 01100572 A CN01100572 A CN 01100572A CN 1124248 C CN1124248 C CN 1124248C
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- musk
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- dregs
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Abstract
The present invention discloses a process for preparing musk xylol by a chemical reaction on waste musk ketone dregs. In the process, secondary waste dregs are used as a raw material, under the action of a sulfuric acid catalyst and a stabilizing agent, the nitration of fuming nitric acid is adopted, crude products precipitated from a reaction mixture are extracted by an oxygen-containing CnHm compound as a solvent and are crystallized to separate out musk xylol, or the reaction mixture is extracted with chlorhydrocarbons as a solvent, and after the solvent is removed form an extracted organic phase, the crude products are extracted with an oxygen-containing CnHmO compound as a solvent and are crystallized to separate out musk xylol. The reaction process of the present invention is simple, the yield of the product can reach 90 to 95%, and the purity of musk xylol can reach higher than 99%.
Description
The present invention relates to a kind of method of handling musk ketone waste residue production musk xylene by chemical reaction.Belong to the deep process technology of chemical method to the musk ketone waste residue.
The a large amount of waste residues that produce in the treating process of musk ketone are called waste residue one time.Contain musk ketone 30-35% in the waste residue, musk xylene 6-8%, dinitrobenzene tertiary butyl m-xylene isomer 56-62%.For the processing of a waste residue, the producer that has in recent years adopts solvent crystallization therefrom to extract the musk ketone of 8-10%, and remaining waste residue is called secondary residue.Owing to have a large amount of dinitrobenzene tertiary butyl m-xylene isomer in the secondary residue, at present it is not also found effective separation method, so secondary residue becomes the environomental pollution source of manufacturer, also cause the production cost of producer to improve simultaneously.
The object of the present invention is to provide a kind of method of handling musk ketone waste residue production musk xylene by chemical reaction.This method reaction process is simple, by reaction dinitrobenzene tertiary butyl m-xylene is converted into musk xylene, produces musk xylene and can reach 90-95%.
For achieving the above object, the present invention is realized by following technical proposals.With the secondary residue is raw material, under catalyzer and function of stabilizer, add elutriation and go out solid through nitration reaction with to the mixture of reaction, by filter, washing obtains thick product, thick product is dissolved in that Crystallization Separation goes out musk xylene among the solvent B; Perhaps to the mixture of nitration reaction, adding solvent orange 2 A extracts, after the organic phase that is rich in Moschus in the extraction liquid removes solvent,, it is characterized in that adding B solvent crystallization separating dimethyl benzene Moschus, catalyzer is a sulfuric acid, stablizer is a hydroxy-containing compounds, and nitrating agent is a nitrosonitric acid, the nitration reaction temperature is-and 15-40 ℃, the mass ratio of sulfuric acid and nitric acid is 0.01: 1-5: 1, and the mass ratio of nitric acid and secondary residue is 1: 1-6: 1; Solvent orange 2 A is chlorinated hydrocarbon C
pH
qCl
k, P=1-2 wherein, q=0-5, k=1-6; Solvent B is C
nH
mThe O oxygenatedchemicals aqueous solution, n=1-3, m=4-8, strength of solution is 10%-100% (mass percent).
Below the present invention is described in detail.
One of gordian technique of the present invention is a nitration reaction.Nitrated process can adopt nitrosonitric acid to make nitrating agent, and sulfuric acid is made catalyzer, adds the stablizer of the hydroxy-containing compounds of trace simultaneously, and initial reaction stage is carried out in lower temperature, along with the carrying out of reaction progressively improved temperature of reaction.Post reaction mixture adds elutriation and goes out solid, and solid washes to neutrality through washing or diluted alkaline and obtains thick product, and thick product is dissolved in C
nH
mCrystallization Separation obtains musk xylene in the O oxygenatedchemicals.Nitration reaction process of the present invention also can adopt chlorinated hydrocarbon earlier secondary residue to be dissolved, and adds the nitration mixture for preparing then and carries out nitration reaction.Be reflected in the stirring and carry out, be easy to controls reaction speed.Post reaction mixture is divided into two-phase, and wherein acid can be used as the in addition recycle of nitrating agent of nitration reaction next time mutually.Contain and obtain thick product after organic phase is deviate from solvent, thick product is dissolved in C
nH
mCrystallization Separation goes out musk xylene in the O oxygenatedchemicals, and the process of nitration reaction can also add hydrochloric ether in nitrated back, can reach the purpose that recycles of spent acid equally.Above-mentioned nitration reaction is complied with the different of used raw material and reaction conditions, and the amount that contains musk xylene and musk ketone in the thick product is also different, and musk ketone content is at 1-15%.
Process of the present invention is simple, and because acid solution can be done and recycle, and liquid waste disposal is easy to administer, and product yield can reach 90-95%, musk xylene purity reaches more than 99%.
With embodiment the present invention is further specified again below.
Embodiment one:
Take by weighing 20 gram secondary residues, measure 20 milliliters of nitrosonitric acids, 10 milliliters in 98% sulfuric acid.Nitric acid is added the four-hole boiling flask that band stirs, begin to stir, add micro-stablizer, under the water-bath cooling conditions, drip sulfuric acid.Controlled temperature is 20 ℃, and gradation adds load weighted secondary residue in half an hour then, and reaction is 5 hours under this temperature, after reaction finishes reaction mixture is added in 200 ml waters, filters, and solid drying is got thick product 22g.The thick product that obtains is joined in 180 milliliters of Virahols, be heated to 50 ℃, filtered while hot is removed impurity, and the filtrate cool to room temperature with the solid drying that obtains, obtains musk xylene 17g (purity is 99%) and mother liquor.
Embodiment two:
Take by weighing the 20g secondary residue, measure 10 milliliters of nitrosonitric acids, 10 milliliters in 98% sulfuric acid, 15 milliliters in circulation spent acid.Nitric acid is added the four-hole boiling flask that band stirs, begin to stir, add micro-stablizer, bathe under the cooling conditions, drip sulfuric acid at cryosel.Controlled temperature is 0 ℃, and gradation adds load weighted secondary residue in half an hour then, and reaction is 2 hours under this temperature, removing cryosel then bathes, at room temperature reacted 2.5 hours, and after reaction finishes, added tetracol phenixin 30ML, stirred 10 minutes, tell organic phase then, solvent is deviate from distillation, gets thick product, adopt Virahol crystallization (with embodiment one) then, obtain musk xylene 16g (purity is 99%) and mother liquor.
Embodiment three:
Take by weighing the 20g secondary residue, be dissolved in 20 milliliters of tetracol phenixin, measure 10 milliliters of nitrosonitric acids, 10 milliliters in 98% sulfuric acid, 15 milliliters in circulation spent acid.Nitric acid and circulation spent acid are added the four-hole boiling flask that band stirs, begin to stir, add micro-stablizer, under the water-bath cooling conditions, drip sulfuric acid.Controlled temperature is 10 ℃, drips the carbon tetrachloride solution of dissolving secondary residue then in half an hour, at room temperature reacts 5 hours, tells organic phase after reaction finishes, and solvent is deviate from distillation, obtains thick product, and refining then, process for purification is with embodiment one.Obtain musk xylene 17.5g (purity is 99%) and mother liquor.
Claims (1)
1. handle the method that the musk ketone waste residue is produced musk xylene by chemical reaction for one kind, with the secondary residue is raw material, under catalyzer and function of stabilizer, pass through nitration reaction and the mixture that reacts is added elutriation and go out solid, by filter, washing obtains thick product, thick product is dissolved in that Crystallization Separation goes out musk xylene among the solvent B; Perhaps to the mixture of nitration reaction, adding solvent orange 2 A extracts, after the organic phase that is rich in Moschus in the extraction liquid removes solvent, add B solvent crystallization separating dimethyl benzene Moschus again, it is characterized in that: catalyzer is a sulfuric acid, and stablizer is a hydroxy-containing compounds, nitrating agent is a nitrosonitric acid, the nitration reaction temperature is-15-40 ℃, and the mass ratio of sulfuric acid and nitric acid is 0.01: 1-5: 1, the mass ratio of nitric acid and secondary residue is 1: 1-6: 1; Solvent orange 2 A is chlorinated hydrocarbon C
pH
qCl
k, P=1-2 wherein, q=0-5, k=1-6; Solvent B is C
nH
mThe O oxygenatedchemicals aqueous solution, n=1-3 wherein, m=4-8, strength of solution is 10%-100% (mass percent).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01100572 CN1124248C (en) | 2001-01-16 | 2001-01-16 | Process for preparing muskxylol by chemical reaction on waste musk ketone dregs |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 01100572 CN1124248C (en) | 2001-01-16 | 2001-01-16 | Process for preparing muskxylol by chemical reaction on waste musk ketone dregs |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1305984A CN1305984A (en) | 2001-08-01 |
| CN1124248C true CN1124248C (en) | 2003-10-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 01100572 Expired - Fee Related CN1124248C (en) | 2001-01-16 | 2001-01-16 | Process for preparing muskxylol by chemical reaction on waste musk ketone dregs |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106748795A (en) * | 2016-11-18 | 2017-05-31 | 天津市安凯特科技发展有限公司 | A kind of Safe production method of ketone musk |
| CN112661650A (en) * | 2020-12-25 | 2021-04-16 | 安徽华业香料股份有限公司 | Method for synthesizing musk xylene from azeotrope of side product of propiolactone |
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2001
- 2001-01-16 CN CN 01100572 patent/CN1124248C/en not_active Expired - Fee Related
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