CN102643173A - Lateral line rectification separation method for organic components of polyethylene glycol, ethylene glycol and ethylene glycol monomethyl ether in crystalline silicon cutting mixing recovery liquid - Google Patents
Lateral line rectification separation method for organic components of polyethylene glycol, ethylene glycol and ethylene glycol monomethyl ether in crystalline silicon cutting mixing recovery liquid Download PDFInfo
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- CN102643173A CN102643173A CN2012101064887A CN201210106488A CN102643173A CN 102643173 A CN102643173 A CN 102643173A CN 2012101064887 A CN2012101064887 A CN 2012101064887A CN 201210106488 A CN201210106488 A CN 201210106488A CN 102643173 A CN102643173 A CN 102643173A
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- ethylene glycol
- monomethyl ether
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Abstract
The invention provides a lateral line rectification separation method for organic components of polyethylene glycol, ethylene glycol and ethylene glycol monomethyl ether in crystalline silicon cutting mixing recovery liquid, which comprises the following steps of: (1) taking moisture-free crystalline silicon cutting mixing recovery liquid as raw material, and pumping into a lateral line fractionating tower; (2) carrying out fraction at 124-125 DEG C in a cutting way on the top of the tower, controlling reflux ratio, and recovering an ethylene glycol monomethyl ether product from the top of the tower to enter into an ethylene glycol monomethyl ether storing tank; (3) carrying out fraction at 195-200 DEG C in a cutting way at the lateral line on the upper part of the tower, exchanging heat by a heat exchanger to be taken as an ethylene glycol product to enter into a storing tank; and (4) reheating material on a tower kettle by a reboiler, controlling the temperature to be in a range of 240 DEG C to 245 DEG C, cooling some material to be taken as a polyethylene glycol product to enter into a polyethylene glycol product storing tank. The method adopts optimized technology parameters, and adopts the lateral line of a single tower to separate three components in the crystalline silicon cutting mixing recovery liquid in a rectifying way. The ethylene glycol monomethyl ether is recovered from the top of the tower, the ethylene glycol is recovered from the lateral line, and the polyethylene glycol is obtained from the tower kettle. Due to single-tower operation, the equipment cost and the energy consumption can be reduced compared with those of the conventional method.
Description
Technical field
The present invention relates to a kind of separation method of chemical industry, particularly a kind of crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid.
Background technology
The silicon chip cutting is the key component in the solar-energy photo-voltaic cell ME.This technology is used to handle the solid silicon ingot of silicon single crystal or polysilicon.Scroll saw is cut into very thin silicon chip then at first the silicon ingot dice.Owing on using, performance index such as the surperficial planeness of solar silicon wafers, cleanliness factor, electroconductibility are had strict requirement; In the cutting process of solar silicon wafers, need to use that hardness is high, granularity is little and the silicon carbide micro-powder of centralized particle diameter as main cutting medium.For silicon carbide micro-powder is uniformly dispersed in working angles; In time take away simultaneously the huge heat of friction that produces in the working angles; Usually need earlier according to a certain percentage silicon carbide micro-powder; Joining with polyoxyethylene glycol (PEG) is in the aqueous solution of dispersion agent, is prepared into the finely dispersed water-soluble solar silicon wafers cutting liquid of silit.
In the online cutting process, owing to broken silicon-carbide particle and silicon grain that the collision between silicon-carbide particle and the silicon rod and friction produce also will be sneaked in the cutting system.Simultaneously, the cutting heat that cutting process produces, the qualitative change that also can cause cutting liquid itself, therefore, cutting liquid must be changed after using several times, so the silicon chip cutting is faced with the recycling problem of a large amount of discarded cutting liquid.The staple of cutting waste mortar is an organism, promptly cuts the staple of liquid: the mixed solution of terepthaloyl moietie, many terepthaloyl moietie, ethylene glycol monomethyl ether, silit (as the abrasive material of cutting liquid) and polysilicon (or silicon single crystal) particle that in cutting process, produces etc.Conventional recovery method is to adopt solid-liquid separation that it is divided into mixed solution and mixed sand earlier; Purifying and recovering respectively again, for mixed solution (form and mainly contain polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether, water), industry in separation method commonly used be earlier the employing multiple-effect evaporation with wherein water sepn; Remaining organic constituent such as need further separate; Adopt two tower atmospheric distillations, first column overhead obtains the light constituent ethylene glycol monomethyl ether, and second tower continuation rectifying is sent in heavy constituent at the bottom of the tower; Second column overhead obtains terepthaloyl moietie, and the tower still obtains polyoxyethylene glycol.
The shortcoming of two tower atmospheric distillations mainly aspect two, the one, adopt two tower flow processs, equipment manufacturing cost and process cost are higher, the 2nd, twice evaporation, energy consumption is bigger than normal.This has also directly influenced the cost of crystalline silicon cutting liquid reclaiming.
Summary of the invention
The purpose of this invention is to provide a kind of crystalline silicon cutting and mix the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid; It is raw material (mass ratio of each component is: polyoxyethylene glycol 85 ~ 95, terepthaloyl moietie 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8) that this method is mixed recovery liquid with the crystalline silicon cutting of having removed moisture; Adopt the rectifying of single tower side line; From cat head extraction ethylene glycol monomethyl ether, from side line extraction terepthaloyl moietie, the tower still obtains polyoxyethylene glycol.The present invention can overcome the above-mentioned deficiency of prior art, and when having guaranteed product quality and yield, equipment manufacturing cost, energy consumption obviously reduce.
The technical scheme of accomplishing the foregoing invention task is: a kind of crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid, it is characterized in that step is following,
⑴. mixing recovery liquid with the crystalline silicon cutting of having removed moisture is raw material (mass ratio of each component is: polyoxyethylene glycol 85 ~ 95, terepthaloyl moietie 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8), with being pumped into the side line rectifying tower;
⑵. cat head cuts 124 ~ 125 ℃ of cuts, the control reflux ratio, the cat head extraction gets into the ethylene glycol monomethyl ether storage tank as the ethylene glycol monomethyl ether product;
Trim the top of column is than being 4:1 ~ 8:1, and optimum value is: 6:1.
⑶. tower top side line cuts 195 ~ 200 ℃ of cuts, after the interchanger heat exchange, gets into the terepthaloyl moietie storage tank as the terepthaloyl moietie product;
⑷. tower still material is heated by reboiler, 240 ~ 245 ℃ of controlled temperature, partial material extraction cooling back gets into the polyoxyethylene glycol finished product storage tank as the polyoxyethylene glycol product.
The technical process of sepn process is seen shown in Figure 1, and device adopts and optimizes processing condition in the sepn process, can obtain high purity ethylene glycol monomethyl ether, terepthaloyl moietie and polyoxyethylene glycol simultaneously after the separation.
Advantage of the present invention: adopt technical process shown in Figure 1 and optimized parameters; Raw material is that the crystalline silicon cutting of having removed moisture mixes that to reclaim liquid be raw material (mass ratio of each component is: polyoxyethylene glycol 85 ~ 95, terepthaloyl moietie 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8), adopts single tower side line rectifying separation three kinds of components wherein.Cat head extraction ethylene glycol monomethyl ether, side line extraction terepthaloyl moietie, tower still obtain polyoxyethylene glycol.Owing to be single tower operation, compare with the common distillating method of two towers that routine is used, practiced thrift equipment cost and energy consumption.
Description of drawings
Fig. 1 is the technical process of side line rectifying separation ethylene glycol monomethyl ether, terepthaloyl moietie, polyoxyethylene glycol.
Embodiment
Table 1 rectifying tower processing condition
| Processing parameter | The T-1 tower |
| Theoretical plate number | 60 |
| The raw material feed entrance point | 45 |
| Side line discharging position | 32 |
| Reflux ratio | 6 |
| Tower top pressure | 1atm |
| Tower top temperature (℃) | 124~125 |
| Side stream temperature (℃) | 195-200 |
| Tower still temperature (℃) | 240~250 |
Burst explanation of table 2 stream
Claims (5)
1. a crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid, it is characterized in that step is following,
⑴. mixing recovery liquid with the crystalline silicon cutting of having removed moisture is raw material, with being pumped into the side line rectifying tower;
⑵. cat head cuts 124 ~ 125 ℃ of cuts, the control reflux ratio, the cat head extraction gets into the ethylene glycol monomethyl ether storage tank as the ethylene glycol monomethyl ether product;
⑶. tower top side line cuts 195 ~ 200 ℃ of cuts, after the interchanger heat exchange, gets into the terepthaloyl moietie storage tank as the terepthaloyl moietie product;
⑷. tower still material is heated by reboiler, 240 ~ 245 ℃ of controlled temperature, partial material extraction cooling back gets into the polyoxyethylene glycol finished product storage tank as the polyoxyethylene glycol product.
2. 1 described crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid according to claims, it is characterized in that, among the described step ⑵, trim the top of column is than being 4:1 ~ 8:1.
3. 2 described crystalline silicon cuttings mix the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid according to claims, it is characterized in that among the described step ⑵, the trim the top of column ratio is for being: 6:1.
4. 1 described crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid according to claims; It is characterized in that; Said " the crystalline silicon cutting of having removed moisture mixes recovery liquid " as raw material, the mass ratio of its each component is: polyoxyethylene glycol 85 ~ 95, terepthaloyl moietie 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8.
5. described crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, terepthaloyl moietie, ethylene glycol monomethyl ether in the liquid according to one of claims 1-4, it is characterized in that described rectifying tower processing condition are theoretical plate number: 60; Raw material feed entrance point: 45; Side line discharging position: 32.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709394A (en) * | 2013-12-06 | 2014-04-09 | 江苏盈天化学有限公司 | Method for preparing hydrophilic polyether polyol by utilization of recycled solar silicon chip cutting liquid |
| CN103724612A (en) * | 2013-12-06 | 2014-04-16 | 江苏盈天化学有限公司 | Method for preparing polyatomic alcohol for hydrolysis-resistant coating by using recovered alcohol and epoxy soybean oil |
| CN104447829A (en) * | 2014-11-14 | 2015-03-25 | 南京大学 | Energy-saving separation method and device of ultrapure triethylene glycol methyl ether borate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101239246A (en) * | 2008-02-20 | 2008-08-13 | 江南大学 | Method for recovering cutting solution from by-product of silicon chip cutting processing |
| CN101492360A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Process for the separation of aqueous phase by-product of fischer-tropsch synthesis reaction |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492360A (en) * | 2008-01-23 | 2009-07-29 | 中国石油化工股份有限公司 | Process for the separation of aqueous phase by-product of fischer-tropsch synthesis reaction |
| CN101239246A (en) * | 2008-02-20 | 2008-08-13 | 江南大学 | Method for recovering cutting solution from by-product of silicon chip cutting processing |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103709394A (en) * | 2013-12-06 | 2014-04-09 | 江苏盈天化学有限公司 | Method for preparing hydrophilic polyether polyol by utilization of recycled solar silicon chip cutting liquid |
| CN103724612A (en) * | 2013-12-06 | 2014-04-16 | 江苏盈天化学有限公司 | Method for preparing polyatomic alcohol for hydrolysis-resistant coating by using recovered alcohol and epoxy soybean oil |
| CN103724612B (en) * | 2013-12-06 | 2016-03-02 | 江苏盈天化学有限公司 | A kind of method utilizing recovery alcohol and epoxy soybean oil to prepare hydrolysis coating polyvalent alcohol |
| CN104447829A (en) * | 2014-11-14 | 2015-03-25 | 南京大学 | Energy-saving separation method and device of ultrapure triethylene glycol methyl ether borate |
| CN104447829B (en) * | 2014-11-14 | 2016-11-30 | 南京大学 | The energy-saving separation method of ultra-pure triethylene glycol methyl ether borate and segregation apparatus |
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