CN102643173B - 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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- CN102643173B CN102643173B CN201210106488.7A CN201210106488A CN102643173B CN 102643173 B CN102643173 B CN 102643173B CN 201210106488 A CN201210106488 A CN 201210106488A CN 102643173 B CN102643173 B CN 102643173B
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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, ethylene glycol, ethylene glycol monomethyl ether in liquid.
Background technology
Silicon chip cutting is the key component in solar-energy photo-voltaic cell manufacturing process.This technique is for the treatment of the solid silicon ingot of silicon single crystal or polysilicon.Scroll saw, first silicon ingot dice, is then cut into very thin silicon chip.Owing in application, the performance index such as the planeness on solar silicon wafers surface, cleanliness factor, electroconductibility being had to 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, take away in time the huge heat of friction producing in working angles simultaneously, conventionally need by silicon carbide micro-powder according to a certain percentage first, join and take in the aqueous solution that polyoxyethylene glycol (PEG) is dispersion agent, be prepared into the finely dispersed water-soluble solar silicon wafers cutting liquid of silicon carbide.
In cutting on line process, because broken silicon-carbide particle and silicon grain that the collision between silicon-carbide particle and silicon rod and friction produce also will be sneaked in cutting system.Meanwhile, the cutting heat that cutting process produces, also can cause the qualitative change of cutting liquid itself, and therefore, cutting liquid must be changed after using several times, so silicon chip cutting is faced with the recycling problem of a large amount of discarded cutting liquids.The main component of cutting waste mortar is organism, be the main component of cutting liquid: the mixed solution of ethylene glycol, many ethylene glycol, ethylene glycol monomethyl ether, silicon carbide (as the abrasive material of cutting liquid), and the polysilicon producing in cutting process (or silicon single crystal) particle etc.Conventional recovery method is first to adopt solid-liquid separation to be divided into mixed solution and mixed sand, purifying reclaims respectively again, for mixed solution (forming main containing polyoxyethylene glycol, ethylene glycol, ethylene glycol monomethyl ether, water), industrial conventional separation method is first to adopt multiple-effect evaporation that water wherein is separated, remaining organic constituent is as further separated in need, adopt two tower atmospheric distillations, First column overhead obtains light constituent ethylene glycol monomethyl ether, at the bottom of tower, heavy constituent is sent to second tower continuation rectifying, second column overhead obtains ethylene glycol, and tower reactor 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 affected the cost of crystalline silicon cutting liquid reclaiming.
Summary of the invention
The object 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, ethylene glycol, ethylene glycol monomethyl ether in liquid, the method be take the crystalline silicon cutting of having removed moisture and is mixed that to reclaim liquid be raw material (mass ratio of each component is: polyoxyethylene glycol 85 ~ 95, ethylene glycol 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8), adopt the rectifying of single tower side line, from overhead extraction ethylene glycol monomethyl ether, from side line extraction ethylene glycol, tower reactor 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 that completes foregoing invention task is: a kind of crystalline silicon cutting mixes the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, ethylene glycol, ethylene glycol monomethyl ether in liquid, it is characterized in that, step is as follows,
(1). the crystalline silicon cutting of having removed moisture of take mixes reclaims liquid as raw material (mass ratio of each component is: polyoxyethylene glycol 85 ~ 95, ethylene glycol 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8), with being pumped into side line rectifying tower;
(2). tower top cuts 124 ~ 125 ℃ of cuts, controls reflux ratio, and overhead extraction is as ethylene glycol monomethyl ether product introduction ethylene glycol monomethyl ether storage tank;
Trim the top of column is than being 4:1 ~ 8:1, and optimum value is: 6:1.
. tower top side line cuts 195 ~ 200 ℃ of cuts, after interchanger heat exchange as ethylene glycol product introduction ethylene glycol storage tank;
(4). tower reactor material is heated by reboiler, controls 240 ~ 245 ℃ of temperature, and partial material extraction is cooling rear as polyoxyethylene glycol product introduction polyoxyethylene glycol finished product storage tank.
As shown in Figure 1, in sepn process, device adopts Optimizing Technical, after separation, can obtain high purity ethylene glycol monomethyl ether, ethylene glycol and polyoxyethylene glycol simultaneously in the technical process of sepn process.
Advantage of the present invention: the processing parameter that adopts technical process shown in Fig. 1 and optimization, 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, ethylene glycol 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8), adopts single tower side line rectifying separation three kinds of components wherein.Overhead extraction ethylene glycol monomethyl ether, side line extraction ethylene glycol, tower reactor obtain polyoxyethylene glycol.Owing to being single tower operation, compare with the common distillating method of two towers that routine is used, saved equipment cost and energy consumption.
Accompanying drawing explanation
Fig. 1 is the technical process of side line rectifying separation ethylene glycol monomethyl ether, ethylene glycol, polyoxyethylene glycol.
Embodiment
Embodiment 1, the cutting of side line rectifying separation crystalline silicon mixes the method that reclaims organic constituent in liquid, with reference to processing parameter shown in technical process shown in Fig. 1 and table 1,1. raw material reclaims liquid for the crystalline silicon cutting after dewatering mixes, and wherein the mass content of ethylene glycol monomethyl ether, ethylene glycol, polyoxyethylene glycol is respectively 5%, 5%, 90%, and flow is 10Kg/h, side line rectifying tower T1 absolute pressure of top of the tower is 1atm, temperature is 124 ~ 125 ℃, and control of reflux ratio is in 6 left and right, overhead extraction thing
flow is 0.5 Kg/h, consists of x
ethylene glycol monomethyl ether=0.9787, x
ethylene glycol=0.0194, x
polyoxyethylene glycol=0.0005, lateral line discharging
, temperature is 195 ~ 200 ℃, flow 0.5 Kg/h, consists of x
ethylene glycol monomethyl ether=0.0127, x
ethylene glycol=0.9789, x
polyoxyethylene glycol=0.0032, tower reactor discharging 4. flow is 9Kg/h, consists of x
ethylene glycol=0.0008, x
polyoxyethylene glycol=0.0012, x
methyl polyoxyethylene glycolin=0.9980, figure, 1 is condenser, and 2 is ethylene glycol monomethyl ether receiving tank, and 3 is water cooler, and 4 is ethylene glycol receiving tank, and 5 is reboiler, and 6 is water cooler, and 7 is polyoxyethylene glycol receiving tank.1.-be 4. stream burst title (table 2).
Table 1 rectifying tower processing condition
| Processing parameter | T-1 tower |
| Theoretical plate number | 60 |
| Raw material feed entrance point | 45 |
| Lateral line discharging position | 32 |
| Reflux ratio | 6 |
| Tower top pressure | 1atm |
| Tower top temperature (℃) | 124~125 |
| Side stream temperature (℃) | 195-200 |
| Tower reactor temperature (℃) | 240~250 |
Burst explanation of table 2 stream
Embodiment 2, substantially the same manner as Example 1, but wherein control of reflux ratio is 4:1.
Embodiment 3, substantially the same manner as Example 1, but wherein control of reflux ratio is 8:1.
Embodiment 4, substantially the same manner as Example 1, but the wherein requirement to the proportion of composing of raw material is slightly relaxed.The technical program equally can be accomplished.
Claims (2)
1. crystalline silicon cutting mixes a side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, ethylene glycol, ethylene glycol monomethyl ether in liquid, it is characterized in that, step is as follows,
(1). the crystalline silicon cutting of having removed moisture of take mixes that to reclaim liquid be raw material, with being pumped into side line rectifying tower;
(2). tower top cuts 124 ~ 125 ℃ of cuts, controls reflux ratio, and overhead extraction is as ethylene glycol monomethyl ether product introduction ethylene glycol monomethyl ether storage tank;
. tower top side line cuts 195 ~ 200 ℃ of cuts, after interchanger heat exchange as ethylene glycol product introduction ethylene glycol storage tank;
(4). tower reactor material is heated by reboiler, controls 240 ~ 245 ℃ of temperature, and partial material extraction is cooling rear as polyoxyethylene glycol product introduction polyoxyethylene glycol finished product storage tank;
Described step (2) in, trim the top of column is than for 4:1 ~ 8:1;
Described " 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, ethylene glycol 5 ~ 10, ethylene glycol monomethyl ether 2 ~ 8;
Described rectifying tower processing condition are, theoretical plate number: 60; Raw material feed entrance point: 45; Lateral line discharging position: 32.
2. according to the crystalline silicon cutting described in claims 1, mix the side line distillation and separation method that reclaims organic constituent polyoxyethylene glycol, ethylene glycol, ethylene glycol monomethyl ether in liquid, it is characterized in that, described step (2) in, trim the top of column ratio is: 6:1.
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| CN103709394B (en) * | 2013-12-06 | 2015-10-14 | 江苏盈天化学有限公司 | A kind of method utilizing recovery solar silicon wafers cutting liquid to prepare polyether glycol |
| 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 |
| 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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