CN100551897C - The refining method of purifying of long alkyl chain methacrylates - Google Patents
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Abstract
The present invention relates to the refining method of purifying of a kind of long alkyl chain methacrylates, its technology comprises: 1. washing: in volume ratio is the described long-chain ester monomer of washing in 1: 2～4: 1 the deionized water, 30～60 ℃ of temperature, washing 1～10min, sedimentation 10～60min; 2. alkali cleaning: it is that 1～20% aqueous sodium hydroxide solution carries out alkali cleaning that the upper strata organic liquor of washing mixed solution is placed mass concentration, 30～60 ℃ of temperature, and the monomeric volume ratio of alkali lye and long-chain ester is 1: 2～4: 1, washs 1～10min, sedimentation 10～60min; 3. salt is washed: it is that 1～20% sodium chloride aqueous solution carries out salt and washes that the upper strata organic liquor after the alkali cleaning is placed mass concentration, and technology is with 2; 4. secondary water washing: the salt washing lotion spends ion-cleaning 3～10 times, and technology makes the pH value of upper strata organic liquor reach neutrality with 1; 5. underpressure distillation: secondary water washing is washed mixed solution leave standstill, behind the separatory,, can obtain the purified long alkyl chain methacrylates in vacuum tightness 10～100kPa, 70～100 ℃ of following underpressure distillation of temperature.
Description
Technical field
The present invention relates to the refining purification techniques of chemical industry synthon, be specially and a kind ofly be intended to improve monomer purity and then improve by the refining method of purifying of the long alkyl chain methacrylates of its synthetic resins oil absorptiveness, international Patent classificating number intends being Int.Cl.C07C 57/00 (2006.01).
Background technology
Along with a large amount of developments and utilizations of petroleum resources, oily resource becomes more and more in short supply, and the trade in oil between country is also more and more frequent.In the process of petroleum resources exploitation and conveying, the leakage of oil incident happens occasionally, and has not only wasted valuable petroleum resources, also very big pollution has been caused in ocean and environment, thereby the emphasis that just becomes various countries' concern and research is handled in leakage of oil.
Oil-absorbing resin provides wide prospect as a kind of functional materials for solving this difficult problem.Methacrylic dodecyl gallate homopolymer and copolymer resin are exactly typical oil-absorbing resin, it has the selection adsorptivity to multiple oil product molecule, thereby the focus that becomes research is [referring to (Dan Guorong etc., the oil absorptive function research of physical crosslinking type high oil absorbing resin, journal of applied, 2003,90:3945-3950.Guo-Rong Shan, Ping-Ying Xu, Zhi-Xue Weng, Zhi-Ming Huang, Oil-Absorption Function ofPhysical Crosslinking in the High-Oil-Absorption Resins[J], Journal of AppliedPolymer Science, 2003,90:3945-3950), (Dan Guorong etc., polyhutadiene fill the synthetic and character of high oil absorbing resin, journal of applied, 2003,89:3309-3314.Guo-Rong Shan, Ping-Ying Xu, Zhi-Xue Weng, Zhi-Ming Huang, Synthesis and Properties of Oil AbsorptionResins Filled with Polybutadiene[J], Journal of Applied Polymer Science, 2003,89:3309-3314), (obturage Xiao Changfa, n-BMA/methacrylic dodecyl gallate copolymerization oil suction fibre research, journal of applied, 2006,101:1248-1251.Y.Feng, C.F.Xiao, Research on Butyl Methacrylate-Lauryl Methacrylate Copolymeric Fibers for OilAbsorbency[J], Journal of Applied Polymer Science, 2006,101:1248-1251), (Xie Xiaohong etc., the copolymerization of long-chain alkyl methacrylates and the research of oil absorptiveness [J] thereof, Inner Mongol University of Technology's journal, 2002,21 (3): 174-177), (Lu Jianmei, Guo Yongwei, Wang Hong, synthetic and the performance study [J] of methacrylic dodecyl gallate and Octyl methacrylate copolymerization high oil-absorbing resin, Suzhou Imperial College journal (natural science), 1995,11 (1): 100-104), (obturage, Xiao Changfa, semi-intercrossing network copolymerization methacrylic ester fiber production and crosslinking structure research [J] thereof, Tianjin University of Technology's journal, 2005,24 (6): 5-7), (Huang Kaibing etc., the synthetic and sign [J] of poly-(vinylbenzene-alkyl methacrylate) high oil absorbing resin, petrochemical complex, 2006,35 (9): 841-845), (Chen Zili etc., the evaluation of polymethyl acrylic acid dodecyl ester and synthetic [J], Ji'nan University's journal (natural science edition), 1994,15 (3): 74-78)].Domestic long alkyl chain methacrylates mostly is technical grade, and the source is wide, low price, but foreign matter content is higher, has shortcomings such as shade deviation, oil suction speed is slow, the oil suction multiplying power is low by its synthetic resin.In recent years along with science and technology development, domesticly also begin to occur other long alkyl chain methacrylates of chemical pure level, but it costs an arm and a leg, and has improved the synthetic and application cost that contains the long alkyl chain methacrylates oil-absorbing resin, is unfavorable for very much commercial scale production and application.Therefore the technical grade long alkyl chain methacrylates is made with extra care, improved its purity, and then improve oil absorption, handle significant leakage of oil by its synthetic resins.
At present, the direct esterification method is adopted in the preparation of methacrylic ester (comprising the methacrylic dodecyl gallate) mostly.Direct esterification method technology is simple, reaction times is short, temperature is lower, easily adopted by people, but in the process of its preparation methacrylate monomer, having methacrylic acid and alcohol remains in the monomer, if do not remove these impurity, in the process of synthetic resins, contain the methacrylic acid meeting polymerization reaction take place of two keys, the wetting ability of itself can reduce the oil absorption of synthetic resins, and residual alcohol also can cause interference to reaction.Therefore, present refining target to methacrylic ester all concentrates on and removes these impurity.For example: Chinese patent literature CN200510029416.7 discloses the synthetic and method of purification of a kind of more function group (methyl) acrylate, this invention is adopted and is mixed entrainer, preferably resolve owing to use single entrainer in esterification process, to cause sticking wall, the problem of product color difference.Its thick product is purified through refining, can get high-quality product, and yield is greater than 95%, and purity is more than 99%, and colourity (APHA) is less than 20.But this method has adopted the mixing entrainer in the process of esterification, improved energy consumption in the distillation stage, mixes entrainer simultaneously and is difficult to separate, and easily causes environmental pollution.In order to solve the drawback that the direct esterification method is brought, Chinese patent literature CN03128484.1 discloses a kind of improving one's methods of methacrylic acid and methacrylic ester that prepare.This method adopts the treatment process of combination or associating, comprises that the treatment step of associating hydrolysis, combination cracking system and combination thereof prepares methacrylic acid and methacrylate monomer.In addition, this method also provides purifying crude methacrylic acid logistics to form the method that purity is at least 95% methacrylic acid.But this method appointed condition requires high, complicated operation, and the industrialization difficulty is bigger.
Summary of the invention
At the deficiencies in the prior art, the technical problem to be solved in the present invention is to design the refining method of purifying of a kind of long alkyl chain methacrylates.This method can improve the chromaticness and the purity of long alkyl chain methacrylates effectively, make refining back long alkyl chain methacrylates synthetic resin oil absorptiveness that outstanding raising be arranged, even meet or exceed the oil absorptiveness of import chemical pure long alkyl chain methacrylates synthetic resins, for handling oil leaking pollution, economize on resources and open up an economic route, it is simple to have technology simultaneously, do not pollute, appointed condition there is not particular requirement, with low cost, be convenient to the characteristics of industrial applications.
The technical scheme that the present invention solve the technical problem is: design the refining method of purifying of a kind of long alkyl chain methacrylates, its technology comprises:
1. washing: it is that 1: 2～4: 1 deionized water for stirring is washed that the technical grade long alkyl chain methacrylates is placed deionized water and technical grade long alkyl chain methacrylates volume ratio, must wash mixed solution, washing temperature is controlled at 30～60 ℃, washing time is controlled at 1～10min, and the settling time is 10～60min;
2. alkali cleaning: above-mentioned washing mixed solution is left standstill, behind the separatory, it is that 1～20% aqueous sodium hydroxide solution carries out alkali cleaning that the upper strata organic liquor is placed mass concentration, get the alkali cleaning mixed solution, the alkali cleaning temperature is 30～60 ℃, aqueous sodium hydroxide solution and the monomeric volume ratio of described long-chain ester are 1: 2～4: 1, and washing time is 1～10min, and the settling time is 10～60min;
3. salt is washed: above-mentioned alkali cleaning mixed solution is left standstill, behind the separatory, it is that 1～20% sodium chloride aqueous solution carries out salt and washes that the upper strata organic liquor is placed mass concentration, get salt and wash mixed solution, it is 30～60 ℃ that salt is washed temperature, sodium chloride aqueous solution and the monomeric volume ratio of described long-chain ester are 1: 2～4: 1, and washing time is 1～10min;
4. secondary water washing: above-mentioned salt is washed mixed solution leave standstill, behind the separatory, at ambient temperature, again the upper strata organic liquor being placed deionized water and the monomeric volume ratio of described long-chain ester is that 1: 2～4: 1 deionized water washs 3～10 times, make the pH value of upper strata organic liquor reach neutrality, get secondary water washing and wash mixed solution;
5. underpressure distillation: above-mentioned secondary water washing being washed mixed solution leave standstill, behind the separatory, is the upper strata organic liquor that 10～100KPa, temperature are under 70～100 ℃ in vacuum tightness, carries out underpressure distillation, promptly obtains the purified long alkyl chain methacrylates.
Compared with prior art, the inventive method because adopted that washing, alkali cleaning, salt are washed, method that secondary water washing and underpressure distillation combine, alkali lye behind the separatory and saline solution can use repeatedly, thereby it is simple to have technology, removal of impurities is thorough, and is with low cost, and it is low to consume energy, save energy, advantage such as environmentally friendly.
Embodiment
Below in conjunction with specific embodiment the inventive method is further elaborated.
The refining method (hereinafter to be referred as method) of purifying of a kind of long alkyl chain methacrylates of the present invention's design (being called for short the long-chain ester monomer), its technology comprises:
1. washing: place deionized water to stir washing certain volume technical grade long-chain ester monomer, temperature is controlled at 30～60 ℃, the monomeric volume ratio of deionized water and long-chain ester is controlled between 1: 2～4: 1, and washing time is controlled at 1～10min, and the settling time is 10～60min.
2. alkali cleaning: above-mentioned mixed solution is left standstill, behind the separatory, place alkali lye to carry out alkali cleaning the upper strata organic liquor, wherein used alkali lye is aqueous sodium hydroxide solution, mass concentration is 1～20%, and the alkali cleaning temperature is 30～60 ℃, and the monomeric volume ratio of alkali lye and long-chain ester is 1: 2～4: 1, washing time is 1～10min, and the settling time is 10～60min.
3. salt is washed: above-mentioned mixed solution is left standstill once more, behind the separatory, placing salts solution to carry out salt the upper strata organic liquor washes, wherein used salt solution is sodium chloride aqueous solution, mass concentration is 1～20%, wash temperature is 30～60 ℃, and the monomeric volume ratio of salts solution and long-chain ester is 1: 2～4: 1, and washing time is～10min;
4. secondary water washing: above-mentioned mixed solution behind the separatory, places deionized water to wash the upper strata organic liquor through leaving standstill, temperature keeps at ambient temperature, the monomeric volume ratio of deionized water and long-chain ester is 1: 2～4: 1, and washing times is 3～10 times, and the pH value of final upper strata organic liquor reaches neutrality;
5. underpressure distillation: above-mentioned mixed solution is left standstill, behind the separatory, carry out underpressure distillation, can obtain the purified long alkyl chain methacrylates.This long-chain ester monomer purity is near chemical pure.
The inventive method is at first washed the technical grade long alkyl chain methacrylates under the certain temperature condition with deionized water, can remove some easy molten impurity, wash being higher than under the room temperature condition simultaneously, can improve the solvability of residual methacrylic acid in water again, and then remove a small amount of methacrylic acid.According to time temperature equivalence principle, when washing, temperature and time is all unsuitable long, otherwise can cause long alkyl chain methacrylates ester generation thermopolymerization, forms oligopolymers such as dimer.The purpose of alkali liquid washing is the remaining methacrylic acid of neutralization, separates and removes neutralized reaction product, in this course, temperature is unsuitable too high, otherwise under the effect of alkali lye, hydrolysis can take place methacrylic ester, same principle, concentration of lye is unsuitable too high, and washing time is also unsuitable oversize.The purpose of saline solution washing is that to improve system density poor, make the not emulsification of mixed solution after alkali lye is handled, easier processing, accelerated the layering of organic phase and water in the mixed solution, pass through salting out simultaneously, reduced the solvability of easy molten impurity in organic phase, in the saline solution washing stage, too high and time of temperature oversize all can the initiator system thermopolymerization, so keep suitable temperature, and for saline solution concentration, help saline solution the carrying out of washing stage more though saline solution concentration is high more, but the too high number of times that can increase the secondary water washing of back of saline solution concentration, even saline solution can remain in the organic phase.Adopt secondary water washing mixed system can be washed till neutrality.In addition, in treating process, the inventive method also can use potassium hydroxide to carry out alkali liquid washing, uses Repone K to carry out the saline solution washing.
The further feature of the inventive method is, all preferred 1: 1 of the volume ratio of described deionized water, aqueous sodium hydroxide solution and sodium chloride aqueous solution and long alkyl chain methacrylates, preferred 50 ℃ of wash temperature, the preferred 5min of washing time, preferred 30min of settling time, aqueous sodium hydroxide solution mass concentration preferred 8% or 10%, sodium chloride aqueous solution mass concentration preferred 10%, preferred 3 times of secondary water washing number of times, preferred 70 ℃ of vacuum distillation temperature, the preferred 15KPa of vacuum tightness.
Provide the specific embodiment of the inventive method below, but embodiment does not limit the present invention.
Embodiment 1
500ml crude methacrylic acid long-chain ester monomer is placed the 2000ml four-hole boiling flask, add the 500ml deionized water, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min, mixed solution is transferred in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask, add mass concentration again and be 2% sodium hydroxide solution 500ml, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min is transferred to mixed solution in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask once more, the adding mass concentration is 10% sodium chloride solution 500ml, at 50 ℃ of stirred in water bath washing 5min, mixed solution is transferred in the separating funnel, leaves standstill, behind the separatory, divide with deionized water and 3 times the upper strata organic liquor to be washed, leave standstill, separatory, the consumption of each deionized water is 500ml, uses the air bubbling at last, carries out underpressure distillation under 70 ℃ of conditions, vacuum tightness is 15KPa, get the purpose product yield greater than 90%, after tested, the monomeric purity of gained long-chain ester is 92%.
Embodiment 2
500ml crude methacrylic acid long-chain ester monomer is placed the 2000ml four-hole boiling flask, add the 500ml deionized water, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min, mixed solution is transferred in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask, add mass concentration again and be 4% sodium hydroxide solution 500ml, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min is transferred to mixed solution in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask once more, the adding mass concentration is 10% sodium chloride solution 500ml, at 50 ℃ of stirred in water bath washing 5min, mixed solution is transferred in the separating funnel, leaves standstill, behind the separatory, divide with deionized water and 3 times the upper strata organic liquor to be washed, leave standstill, separatory, the consumption of each deionized water is 500ml, uses the air bubbling at last, carries out underpressure distillation under 70 ℃ of conditions, vacuum tightness is 15KPa, get the purpose product yield greater than 90%, after tested, the monomeric purity of gained long-chain ester is 93%.
Embodiment 3
500ml crude methacrylic acid long-chain ester monomer is placed the 2000ml four-hole boiling flask, add the 500ml deionized water, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min, mixed solution is transferred in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask, add mass concentration again and be 6% sodium hydroxide solution 500ml, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min is transferred to mixed solution in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask once more, the adding mass concentration is 10% sodium chloride solution 500ml, at 50 ℃ of stirred in water bath washing 5min, mixed solution is transferred in the separating funnel, leaves standstill, behind the separatory, divide with deionized water and 3 times the upper strata organic liquor to be washed, leave standstill, separatory, the consumption of each deionized water is 500ml, uses the air bubbling at last, carries out underpressure distillation under 70 ℃ of conditions, vacuum tightness is 15KPa, get the purpose product yield greater than 90%, after tested, the monomeric purity of gained long-chain ester is 95%.
Embodiment 4
500ml crude methacrylic acid long-chain ester monomer is placed the 2000ml four-hole boiling flask, add the 500ml deionized water, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min, mixed solution is transferred in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask, add mass concentration again and be 8% sodium hydroxide solution 500ml, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min is transferred to mixed solution in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask once more, the adding mass concentration is 10% sodium chloride solution 500ml, at 50 ℃ of stirred in water bath washing 5min, mixed solution is transferred in the separating funnel, leaves standstill, behind the separatory, divide with deionized water and 3 times the upper strata organic liquor to be washed, leave standstill, separatory, the consumption of each deionized water is 500ml, uses the air bubbling at last, carries out underpressure distillation under 70 ℃ of conditions, vacuum tightness is 15KPa, get the purpose product yield greater than 90%, after tested, the monomeric purity of gained long-chain ester is 97%.
Embodiment 5
500ml crude methacrylic acid long-chain ester monomer is placed the 2000ml four-hole boiling flask, add the 500ml deionized water, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min, mixed solution is transferred in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask, add mass concentration again and be 10% sodium hydroxide solution 500ml, at 50 ℃ of stirred in water bath washing 5min, sedimentation 30min is transferred to mixed solution in the separating funnel, leave standstill, behind the separatory, the upper strata organic liquor is poured in the four-hole boiling flask once more, the adding mass concentration is 10% sodium chloride solution 500ml, at 50 ℃ of stirred in water bath washing 5min, mixed solution is transferred in the separating funnel, leaves standstill, behind the separatory, divide with deionized water and 3 times the upper strata organic liquor to be washed, leave standstill, separatory, the consumption of each deionized water is 500ml, uses the air bubbling at last, carries out underpressure distillation under 70 ℃ of conditions, vacuum tightness is 15KPa, get the purpose product yield greater than 90%, after tested, the monomeric purity of gained long-chain ester is 98%.
Positively effect for check the inventive method, conventional industry level long alkyl chain methacrylates of long alkyl chain methacrylates, worker and import chemical pure long alkyl chain methacrylates after the contriver makes with extra care with embodiment 1-5 gained respectively are monomer, carried out the experiment of contrast synthetic resins, and the oil absorptiveness of having tested institute's synthetic resins.Experimental technique and test result are as follows:
Resin is synthetic:
In the 250ml four-hole boiling flask, add polyethylene of dispersing agent alcohol (PVA) 0.1736g and 120ml deionized water, fully after the dissolving, 40ml long alkyl chain methacrylates, 0.1736g benzoyl peroxide (BPO) are added in the beaker, be stirred to the formation homogeneous solution, then this solution added in the four-hole boiling flask, feed nitrogen, stirring is warming up to 75 ℃, behind the reaction 4h, be increased to 85 ℃, after continuing to react 2h, termination reaction, take out product, washing, drying promptly get white synthetic resins.
Saturated oil absorbency test:
Accurately take by weighing the 1g oil-absorbing resin, in the polyester non-woven fabric bag of packing into, be immersed in the oil product to be measured, normal temperature soaks 24h down, and filtration takes by weighing its total mass after removing unabsorbed oil; Simultaneously, the empty bag of the polyester non-woven fabric after the oil suction is carried out same mensuration, is calculated as follows saturated oil absorbency then:
Saturated oil absorbency=
(empty bag quality after cloth bag total mass-resin quality (1g)-oil suction)/resin quality (1g).
Be that the oil absorptiveness test result example of monomer synthetic resins is in table 1 with embodiment 1-5 gained long alkyl chain methacrylates, technical grade long alkyl chain methacrylates and import chemical pure long alkyl chain methacrylates respectively.In table 1, embodiment is numbered 0 the common comparative example who does not have purified long alkyl chain methacrylates synthetic resins that is; Embodiment be numbered 6 for the comparative example of import chemical pure long alkyl chain methacrylates synthetic resins.By table 1 measured data as can be seen, long alkyl chain methacrylates after the inventive method is refining, its purity is the highest can to reach 98%, be significantly improved by its synthetic resin oil absorption, through preferred parameter purified long alkyl chain methacrylates, behind the synthetic resins, its oil absorption has met or exceeded the chemical pure long alkyl chain methacrylates synthetic of import resin, but the cost that the inventive method spent only is to buy 5% of the chemical pure long alkyl chain methacrylates of import, cost significantly reduces, be very suitable for industrialization promotion and use, have remarkable economic efficiency.
The saturated oil absorbency contrast table of table 1 long alkyl chain methacrylates synthetic resins
Claims (2)
1. a long alkyl chain methacrylates is made with extra care the method for purifying, and its technology comprises:
(1). washing: it is that 1: 2～4: 1 deionized water for stirring is washed that the technical grade long alkyl chain methacrylates is placed deionized water and technical grade long alkyl chain methacrylates volume ratio, must wash mixed solution, washing temperature is controlled at 30～60 ℃, washing time is controlled at 1～10min, and the settling time is 10～60min;
(2). alkali cleaning: above-mentioned washing mixed solution is left standstill, behind the separatory, it is that 1～20% aqueous sodium hydroxide solution carries out alkali cleaning that the upper strata organic liquor is placed mass concentration, get the alkali cleaning mixed solution, the alkali cleaning temperature is 30～60 ℃, aqueous sodium hydroxide solution and the monomeric volume ratio of described long-chain ester are 1: 2～4: 1, and washing time is 1～10min, and the settling time is 10～60min;
(3). salt is washed: above-mentioned alkali cleaning mixed solution is left standstill, behind the separatory, it is that 1～20% sodium chloride aqueous solution carries out salt and washes that the upper strata organic liquor is placed mass concentration, get salt and wash mixed solution, it is 30～60 ℃ that salt is washed temperature, sodium chloride aqueous solution and the monomeric volume ratio of described long-chain ester are 1: 2～4: 1, and washing time is 1～10min;
(4). secondary water washing: above-mentioned salt is washed mixed solution leave standstill, behind the separatory, at ambient temperature, again the upper strata organic liquor being placed deionized water and the monomeric volume ratio of described long-chain ester is that 1: 2～4: 1 deionized water washs 3～10 times, make the pH value of upper strata organic liquor reach neutrality, get secondary water washing and wash mixed solution;
(5). underpressure distillation: above-mentioned secondary water washing being washed mixed solution leave standstill, behind the separatory, is the upper strata organic liquor that 10～100KPa, temperature are under 70～100 ℃ in vacuum tightness, carries out underpressure distillation, promptly obtains the purified long alkyl chain methacrylates.
2. the refining method of purifying of long alkyl chain methacrylates according to claim 1, the volume ratio that it is characterized in that described deionized water, aqueous sodium hydroxide solution and sodium chloride aqueous solution and long alkyl chain methacrylates is 1: 1, wash temperature is 50 ℃, washing time is 5min, settling time is 30min, the aqueous sodium hydroxide solution mass concentration is 8% or 10%, the sodium chloride aqueous solution mass concentration is 10%, the secondary water washing number of times is 3 times, vacuum distillation temperature is 70 ℃, and vacuum tightness is 15KPa.
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