CN101434606B - Polypropylene transparent nucleating agent production method - Google Patents
Polypropylene transparent nucleating agent production method Download PDFInfo
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- CN101434606B CN101434606B CN2008102199781A CN200810219978A CN101434606B CN 101434606 B CN101434606 B CN 101434606B CN 2008102199781 A CN2008102199781 A CN 2008102199781A CN 200810219978 A CN200810219978 A CN 200810219978A CN 101434606 B CN101434606 B CN 101434606B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
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Abstract
The invention discloses a transparent polypropylene nucleating agent which is bis-chlorophenyl benzylidene sorbitol prepared by the aldol condensation of raw materials of sorbitol and p-chlorobenzaldehyde under the action of a single solvent and an acid ether complex catalyst. The invention also discloses a production method of the transparent polypropylene nucleating agent, comprising the steps of chemosynthesis, solvent recovery, water emulsion system refining, and the like. The transparent polypropylene nucleating agent is tasteless, non-toxic, and has excellent performance. The preparation method provides convenience for solvent recovery and is favorable to the safety of production environment, simualranuously, reduces raw material consumption. The complex catalyst is prepared by organic acid and ether compounds according to the characteristics of the reaction system, thus being beneficial to the full contact between reactants and the catalyst, improving reaction rate and selectivity, and realizing production rate up to more than 92 percent. The new technology adopted by the invention for getting rid of aldehyde odor by water emulsion can produce a transparent nucleating agentproduct which has p-chloro structure, no aldehyde odor and high whiteness by adopting a method for eliminating the aldehyde odor in a water emulsion system, and passes the FDA authentication.
Description
Technical field
The present invention relates to the production method of polypropylene CHJ-1 transparent nucleater, particularly relating to 4-chloro-benzaldehyde and sorbyl alcohol is raw material, with the production method of utilizing water and milk system refining product after single solvent and synthetic two chloro-phenyl-benzylidene sorbitol (CHJ-1) nucleators of composite catalyst again.
Background technology
Sorbitol acetal class polypropylene transparent nucleater is a kind ofly can improve the transparency of plain polypropylene and the lower concentration additive of comprehensive mechanical property.In recent years, nucleator has become one of important additives for plastics, in numerous nucleator kinds, be used for the polypropylene transparent modified effect best be dibenzal sorbitol (DBS) class because the smell problem, use to be subjected to many restrictions.
Summary of the invention
Purpose of the present invention provides a kind of production method by raw material sorbyl alcohol and 4-chloro-benzaldehyde two chloro-phenyl-benzylidene sorbitol polypropylene transparent nucleaters that aldol condensation forms under single solvent and the effect of sour ether composite catalyst.
The technical solution adopted for the present invention to solve the technical problems is:
A kind of production method of polypropylene transparent nucleater is characterized in that this polypropylene nucleater is that molecular formula is: C by raw material sorbyl alcohol and 4-chloro-benzaldehyde two chloro-phenyl-benzylidene sorbitols that aldol condensation forms under single solvent and the effect of sour ether composite catalyst
20H
20O
6Cl
2, structural formula is:
Concrete production stage is as follows: a), chemosynthesis synthesizes being furnished with temperature measurer, stirring rake, organic carrier electric heating system and having in the reactor of water-and-oil separator reflux exchanger, at first in reactor, add 4-chloro-benzaldehyde (A) and Neosorb (B), add the solvent hexanaphthene again, tighten hand hole plate; Open the reactor stirring motor and stir, open the electrical heater heating again, keep 60 ± 5 ℃ of oil temperature, make A expect that dissolving fully and B material mix, behind the A material CL, slowly add sour ether composite catalyst again, described acid is Phenylsulfonic acid or C
1 ~ 12Alkyl benzene sulphonate (ABS), described ether is glycol dimethyl ether or ethylene glycol diethyl ether or butyl glycol ether, opens the cooling-water machine system; Readjust electrically heated furnace oil temperature, make the oil temperature constant at 100～120 ℃, make hexanaphthene in reflux exchanger pump around circuit constantly, the minimum boiling point azcotrope that the water that it and aldol reaction generate forms is constantly taken water out of after reflux exchanger oily water separation, reaction is carried out smoothly, when aquifer yield reached preset value, reaction finished, and thick product generates; B), after the solvent recuperation building-up reactions finishes, electrically heated furnace oil temperature is transferred to 60 ± 5 ℃, utilize waste heat to begin the distillating recovering solvent hexanaphthene this moment, when the solvent quantity of distillate reduces, open vacuum system, suitably decompression stays thick product in the reactor till hexanaphthene steams to the greatest extent; C) the water and milk system refining in stainless steel cask, adds water with thick transferred product, after dispersion machine disperses after colloidal mill, drip washing in whizzer, dehydration then; Thick product through dehydration changes in the stainless steel cask again, adds alkali, and high-speed stirring adds oxygenant to pulp, stirs washing then, centrifuge dehydration 3～4 hours; Drying is beaten powder, the packing of product.
Described alkali can adopt potassium hydroxide or yellow soda ash or sodium hydroxide, and described oxygenant can adopt hydrogen peroxide or clorox.
Wherein, the consumption portion rate of 4-chloro-benzaldehyde and sorbyl alcohol is 105～115/62～75; Acid ether consumption portion rate is 2.6-3.5/3.6-4.5.
R in the two chloro-phenyl-benzylidene sorbitol structural formulas of polypropylene transparent nucleater, the implication of S are: according to the configuration representation of stereochemistry chiral centre, rule is used R, the configuration of S symbolic representation chiral atom in order, arranged clockwise is the R type, and contrary arranged clockwise is the S type.
The physical properties of polypropylene nucleater of the present invention:
A) outward appearance is a white powder, odorlessness, and fineness 200 orders are greater than 98%, and whiteness is greater than 95%.
B) bulk density≤0.3g/cm
3
C) fusing point: 223 ~ 230 ℃
D) purity: 96.8%.
Polypropylene nucleater company standard of the present invention is estimated
Through Guangzhou Product Quality Testing Institute's check, product meets company standard Q/ (HG) CH1-2003 " CHJ-1 polypropylene transparent nucleater ".In addition, CHJ-1 is from whiteness, smell, and aspects such as granularity reach or part index number surpasses the performance of external like product.
The wholesomeness evaluation of polypropylene nucleater product of the present invention
Through the check of sanitary inspection center, Guangdong Province, the LD of CHJ-1 nucleator
50Be 21.5g/Kg.Belong to nontoxic level material.Plastic packing product meets food hygienic standard (GB-9688-88).Also by the SGS check, its result is lead content 2ppm to product, cadmium content N.D simultaneously---do not examine (＜2ppm).Meet food sanitation and use standard.
The invention has the beneficial effects as follows: polypropylene transparent nucleater of the present invention, product is tasteless, nontoxic, excellent property.Production method of the present invention is with single C6 medium and complex catalyst system.The advantage of single medium is the safety that makes things convenient for solvent recuperation and help production environment, reduces material loss simultaneously.Composite catalyst is the characteristics according to reaction system, is made into organic acid and ether compound, helps fully contacting of reactant and catalyzer, has improved speed of reaction and selectivity, and productive rate is up to more than 92%; Because it is very big to the transparent nucleater product odour of chlorine structure, be difficult to remove, do not authenticate by FDA always, the water and milk aldehydes removal stink new technology that the present invention adopts, by adopting the aldehydes removal flavor method of water and milk system, produce the transparent nucleater product that no aldehyde is distinguished the flavor of, whiteness is high, and passed through FDA authentication (FCN No.828) the chlorine structure.
The present invention is further described below in conjunction with embodiment.
Embodiment
Get the raw materials ready: it is standby to get Neosorb, 4-chloro-benzaldehyde, solvent hexanaphthene, yellow soda ash, potassium hydroxide, sodium hydroxide, hydrogen peroxide, clorox, sour ether catalyst.
Embodiment 1
A), chemosynthesis is synthesized being furnished with temperature measurer, stirring rake, organic carrier electric heating system and having in the 1000L reactor of water-and-oil separator reflux exchanger, at first in reactor, add the 4-chloro-benzaldehyde (A) of 105～115kg and the Neosorb (B) of 62～75kg, add the solvent hexanaphthene of about 500-600L again, tighten hand hole plate; Open the reactor stirring motor and stir, open the electrical heater heating again, keep 55 ℃ of oil temperature, make A expect that dissolving fully and B material mix, and need 30 minutes approximately; After confirming A material CL, slowly add Phenylsulfonic acid/ethylene glycol monomethyl ether composite catalyst again, its consumption is Phenylsulfonic acid 2.6-3.5kg/ ethylene glycol monomethyl ether 3.6-4.5kg, after adding in about 10 minutes, opens the cooling-water machine system; Readjust electrically heated furnace oil temperature, make the oil temperature constant at 100～120 ℃, make hexanaphthene in reflux exchanger pump around circuit constantly, the minimum boiling point azcotrope that the water that it and aldol reaction generate forms is constantly taken water out of after reflux exchanger oily water separation, reaction is carried out smoothly, and when aquifer yield reached preset value, reaction finished, thick product generates about 4～4.5 hours consuming time;
B), after the solvent recuperation building-up reactions finishes, electrically heated furnace oil temperature is transferred to 55 ℃, utilize waste heat to begin the distillating recovering solvent hexanaphthene this moment, when the solvent quantity of distillate reduces, open vacuum system, suitably decompression stays thick product in the reactor till hexanaphthene steams to the greatest extent; C) the water and milk system refining in stainless steel cask, adds water with thick transferred product, after dispersion machine disperses after colloidal mill, drip washing in whizzer, dehydration then; Thick product through dehydration changes in the stainless steel cask again, adds 2-4kg NaOH, and high-speed stirring adds 22-35kg H again to pulp
2O
2(H
2O
2Concentration is about 30%), stirred 3～4 hours, and then washing, centrifuge dehydration repeats twice; Drying is beaten powder, the packing of product.
Embodiment 2
A), chemosynthesis is synthesized being furnished with temperature measurer, stirring rake, organic carrier electric heating system and having in the 1000L reactor of water-and-oil separator reflux exchanger, at first in reactor, add the 4-chloro-benzaldehyde (A) of 105～115kg and the Neosorb (B) of 62～75kg, add the solvent hexanaphthene of about 500-550L again, tighten hand hole plate; Open the reactor stirring motor and stir, open the electrical heater heating again, keep 60 ℃ of oil temperature, make A expect that dissolving fully and B material mix, and need 30 minutes approximately; After confirming A material CL, slowly add toluene sulfonic acide/glycol dimethyl ether composite catalyst again, its consumption is toluene sulfonic acide 2.6-3.5kg/ glycol dimethyl ether 3.6-4.5kg, after adding in about 10 minutes, opens the cooling-water machine system; Readjust electrically heated furnace oil temperature, make the oil temperature constant at 100～120 ℃, make hexanaphthene in reflux exchanger pump around circuit constantly, the minimum boiling point azcotrope that the water that it and aldol reaction generate forms is constantly taken water out of after reflux exchanger oily water separation, reaction is carried out smoothly, and when aquifer yield reached preset value, reaction finished, thick product generates about 4～4.5 hours consuming time;
B), after the solvent recuperation building-up reactions finishes, electrically heated furnace oil temperature is transferred to 60 ℃, utilize waste heat to begin the distillating recovering solvent hexanaphthene this moment, when the solvent quantity of distillate reduces, open vacuum system, suitably decompression stays thick product in the reactor till hexanaphthene steams to the greatest extent; C) the water and milk system refining in stainless steel cask, adds water with thick transferred product, after dispersion machine disperses after colloidal mill, drip washing in whizzer, dehydration then; Thick product through dehydration changes in the stainless steel cask again, adds 2-4kg KOH, and high-speed stirring adds the 22-35kg clorox again to pulp, stirred 3～4 hours, and then washing, centrifuge dehydration repeats twice; Drying is beaten powder, the packing of product.
Embodiment 3
A), chemosynthesis is synthesized being furnished with temperature measurer, stirring rake, organic carrier electric heating system and having in the 1000L reactor of water-and-oil separator reflux exchanger, at first in reactor, add the 4-chloro-benzaldehyde (A) of 105～115kg and the Neosorb (B) of 62～75kg, add the solvent hexanaphthene of about 500-600L again, tighten hand hole plate; Open the reactor stirring motor and stir, open the electrical heater heating again, keep 65 ℃ of oil temperature, make A expect that dissolving fully and B material mix, and need 30 minutes approximately; After confirming A material CL, slowly add tosic acid/ethylene glycol dibutyl ether composite catalyst again, its consumption is tosic acid 2.6-3.5kg/ ethylene glycol dibutyl ether 3.6-4.5kg, after adding in about 10 minutes, opens the cooling-water machine system; Readjust electrically heated furnace oil temperature, make the oil temperature constant at 100～120 ℃, make hexanaphthene in reflux exchanger pump around circuit constantly, the minimum boiling point azcotrope that the water that it and aldol reaction generate forms is constantly taken water out of after reflux exchanger oily water separation, reaction is carried out smoothly, and when aquifer yield reached preset value, reaction finished, thick product generates about 4～4.5 hours consuming time;
B), after the solvent recuperation building-up reactions finishes, electrically heated furnace oil temperature is transferred to 65 ℃, utilize waste heat to begin the distillating recovering solvent hexanaphthene this moment, when the solvent quantity of distillate reduces, open vacuum system, suitably decompression stays thick product in the reactor till hexanaphthene steams to the greatest extent; C) the water and milk system refining in stainless steel cask, adds water with thick transferred product, after dispersion machine disperses after colloidal mill, drip washing in whizzer, dehydration then; Thick product through dehydration changes in the stainless steel cask again, adds 2-4kg yellow soda ash, and high-speed stirring adds 22-35kg H again to pulp
2O
2(H
2O
2Concentration is about 30%), stirred 3～4 hours, and then washing, centrifuge dehydration repeats twice; Drying is beaten powder, the packing of product.
Embodiment 4
The processibility of polypropylene nucleater of the present invention and modified performance evaluation
Get the polypropylene nucleater (CHJ-1) that embodiment 1 makes and add processing PP goods among the PP, it is all very good to aspects such as polyacrylic nucleogenesis, optical property, physical and mechanical property modifications, the plastic working that is adapted in 220～240 ℃ of temperature ranges is used, and can satisfy the injection moulding of homopolymerization, Co-polypropylene, the production requirement of extruding, squeezing multiple PP goods such as stretch blow.See table 1 and table 2 data for details.
Table 1 polypropylene nucleater CHJ-1 improve PP optical performance data (with external nucleator product relatively, addition 0.3% is in PP (F401), 1mm injection moulding disk)
Table 2 polypropylene nucleater CHJ-1 is to the improvement (comparing with external nucleator product) of PP (T30S) physical and mechanical properties
By the foregoing description the present invention is had been described in detail, these specify and should be interpreted as only exemplifying, and embodiment of the present invention should not be limited.
Claims (3)
1. the production method of a polypropylene transparent nucleater, it is characterized in that this polypropylene nucleater is that molecular formula is: C by raw material sorbyl alcohol and 4-chloro-benzaldehyde two chloro-phenyl-benzylidene sorbitols that aldol condensation forms under single solvent and the effect of sour ether composite catalyst
20H
20O
6Cl
2, structural formula is:
Concrete production stage is as follows: a), chemosynthesis synthesizes being furnished with temperature measurer, stirring rake, organic carrier electric heating system and having in the reactor of water-and-oil separator reflux exchanger, at first in reactor, add 4-chloro-benzaldehyde (A) and Neosorb (B), add the solvent hexanaphthene again, tighten hand hole plate; Open the reactor stirring motor and stir, open the electrical heater heating again, keep 60 ± 5 ℃ of oil temperature, make A expect that dissolving fully and B material mix, behind the A material CL, slowly add sour ether composite catalyst again, described acid is Phenylsulfonic acid or C
1 ~ 12Alkyl benzene sulphonate (ABS), described ether is glycol dimethyl ether or ethylene glycol diethyl ether or butyl glycol ether, opens the cooling-water machine system; Readjust electrically heated furnace oil temperature, make the oil temperature constant at 100～120 ℃, make hexanaphthene in reflux exchanger pump around circuit constantly, the minimum boiling point azcotrope that the water that it and aldol reaction generate forms is constantly taken water out of after reflux exchanger oily water separation, reaction is carried out smoothly, when aquifer yield reached preset value, reaction finished, and thick product generates; B), after the solvent recuperation building-up reactions finishes, electrically heated furnace oil temperature is transferred to 60 ± 5 ℃, utilize waste heat to begin the distillating recovering solvent hexanaphthene this moment, when the solvent quantity of distillate reduces, open vacuum system, suitably decompression stays thick product in the reactor till hexanaphthene steams to the greatest extent; C) the water and milk system refining in stainless steel cask, adds water with thick transferred product, after dispersion machine disperses after colloidal mill, drip washing in whizzer, dehydration then; Thick product through dehydration changes in the stainless steel cask again, adds alkali, and high-speed stirring adds oxygenant to pulp, stirs washing then, centrifuge dehydration 3～4 hours; Drying is beaten powder, the packing of product.
2. the production method of a kind of polypropylene transparent nucleater according to claim 1 is characterized in that described alkali is potassium hydroxide or yellow soda ash or sodium hydroxide, and described oxygenant is hydrogen peroxide or clorox.
3. the production method of a kind of polypropylene transparent nucleater according to claim 1, it is characterized in that: wherein, the consumption portion rate of 4-chloro-benzaldehyde and sorbyl alcohol is 105～115/62～75; Acid ether consumption portion rate is 2.6-3.5/3.6-4.5.
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|---|---|---|---|
| CN2008102199781A CN101434606B (en) | 2008-12-15 | 2008-12-15 | Polypropylene transparent nucleating agent production method |
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| CN2008102199781A CN101434606B (en) | 2008-12-15 | 2008-12-15 | Polypropylene transparent nucleating agent production method |
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| CN101434606B true CN101434606B (en) | 2011-02-16 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102675331B (en) * | 2012-05-11 | 2014-09-03 | 广州呈和科技有限公司 | Method for producing transparent sorbitol acetal polypropylene nucleating agent |
| CN106795326B (en) * | 2016-09-05 | 2019-01-11 | 呈和科技股份有限公司 | A kind of transparent nucleater composition comprising three acetal of sorbierite and monoacetal |
| CN106317451B (en) | 2016-09-05 | 2019-02-12 | 呈和科技股份有限公司 | A kind of nucleating agent compositions comprising three acetal of micro aromatic aldehyde, two acetal of sorbierite and sorbierite |
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Assignee: GCH Technology Co.,Ltd. Assignor: Zhao Wenlin Contract record no.: 2010440001555 Denomination of invention: Method for producing transparent sorbitol acetal polypropylene nucleating agent License type: Exclusive License Open date: 20090520 Record date: 20101229 |
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Effective date of registration: 20151023 Address after: 510540 Guangzhou Province, Baiyun District, North Road, No. 1633, Guangzhou private science and Technology Park Road, No. 2, No. Patentee after: GCH Technology Co.,Ltd. Address before: 510000, No. 2, strong road, Guangzhou private science and Technology Park, 1633 North Road, Baiyun District, Guangdong, Guangzhou Patentee before: Zhao Wenlin |
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Address after: 510540 Guangzhou Province, Baiyun District, North Road, No. 1633, Guangzhou private science and Technology Park Road, No. 2, No. Patentee after: GCH TECHNOLOGY Co.,Ltd. Address before: 510540 Guangzhou Province, Baiyun District, North Road, No. 1633, Guangzhou private science and Technology Park Road, No. 2, No. Patentee before: Guangdong Chenghe Science and Technology Co.,Ltd. Address after: 510540 Guangzhou Province, Baiyun District, North Road, No. 1633, Guangzhou private science and Technology Park Road, No. 2, No. Patentee after: Guangdong Chenghe Science and Technology Co.,Ltd. Address before: 510540 Guangzhou Province, Baiyun District, North Road, No. 1633, Guangzhou private science and Technology Park Road, No. 2, No. Patentee before: GCH Technology Co.,Ltd. |