CN103450007A - Method for recovering lactic acid from waste lactic acid generated in silicon slice degumming procedure - Google Patents
Method for recovering lactic acid from waste lactic acid generated in silicon slice degumming procedure Download PDFInfo
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Abstract
The invention relates to a method for recovering lactic acid from waste lactic acid generated in a silicon slice degumming procedure. The method comprises the following steps: firstly adding a decolorizing agent to the waste lactic acid; then carrying out solid-liquid separation by using a physical method, and then removing impurities through ion exchange resin; finally concentrating to obtain a finished product by using a double-effect or triple-effect evaporator. The method disclosed by the invention can be used for effectively recovering the lactic acid contained in the waste lactic acid generated in the silicon slice degumming procedure and is high in recovery rate and less in environment pollution. According to the invention, the recovered lactic acid can be continuously used for silicon slice degumming or used for the nickel plating industry, the tanning industry, the cleaning industry, and the like, so that the enterprise production cost of silicon slice cutting and the like can be outstandingly reduced, and the great environment pollution caused by discharging the waste lactic acid is prevented.
Description
Technical field
The invention belongs to useless lactic acid recovery technology field, relate to a kind of method that reclaims lactic acid, reclaim the method for lactic acid especially a kind of useless lactic acid produced from the silicon wafer stripping operation.
Background technology
Lactic acid is a kind of very important organic acid.Industrial production lactic acid mainly adopts microbe fermentation method, mostly take the grains such as corn, sweet potato, starch at China's fermentation raw material as main.The advantages such as lactic acid is easy to use owing to having, and the speed of coming unstuck is fast are widely used in solar silicon wafers comes unstuck.Development along with photovoltaic industry and semiconductor industry, the usage quantity of silicon single crystal and polysilicon constantly increases, especially in recent years the sun power industry constantly increases the demand of big area thin silicon sheet, and lactic acid is at the consumption of photovoltaic industry also cumulative year after year.
Will carry out pre-washing and come unstuck after industrial silicon chip well cutting, the glue on silicon chip can be softening in certain temperature range, and silicon chip comes off from the crystalline substance holder automatically afterwards.When coming unstuck, use lactic acid to reduce and come unstuck temperature and shorten the gum softening time, thereby reduce the silicon chip surface reactivity, enhance productivity, therefore in the silicon wafer stripping operation, lactic acid is used in a large number.But, along with the prolongation of duration of service, the impurity of sneaking in lactic acid can get more and more, concentration constantly descends simultaneously, causes the speed of coming unstuck obviously to reduce.Therefore need constantly add or more renew lactic acid, and then produced the useless lactic acid of a large amount of silicon wafer strippings.Will expend a large amount of grain owing to producing lactic acid, the lactic acid harmless treatment cost that will give up is higher, and it is highly significant that the useless lactic acid therefore the silicon wafer stripping operation produced is recycled research.
Have adhesive tape, blob of viscose etc. and fall into lactic acid when with lactic acid, silicon chip being come unstuck, after the cutting, through a small amount of cutting waste mortar residual on the silicon chip rinsed and water etc., also can bring in lactic acid, iron meeting and the lactic acid reaction of wherein cutting in waste mortar generate iron lactate, ironic lactate etc. simultaneously.Current disclosed periodical, patent, handbook and books etc. are all without the data of the useless lactic acid recovery aspect after silicon wafer stripping.Silicon chip cutting enterprise is mainly stack temporarily or send sewage work to process to the disposal way of useless lactic acid at present, reclaims as can be seen here lactic acid in useless lactic acid for the saving of lactic acid resource and effectively utilizes significant.
Summary of the invention
The object of the invention is to address the above problem, a kind of method that reclaims lactic acid useless lactic acid produced from the silicon wafer stripping operation is provided, the method is that the mode by physical sepn realizes the recycling again to lactic acid in the useless lactic acid after silicon wafer stripping, and the lactic acid after simultaneously making to reclaim can meet the service requirements of silicon wafer stripping operation or the industries such as nickel plating, process hides and cleaning.
In order to achieve the above object, the technical solution adopted in the present invention comprises the following steps:
1) decolouring and separating solid substances:
In useless lactic acid, add discoloring agent to be decoloured, the add-on of discoloring agent is 0.05～5% of useless lactic acid quality, then carries out solid-liquid separation and remove solids, obtains preliminary removal of impurities liquid;
2) decationize impurity:
The liquid of preliminary removal of impurities, by cation exchange resin column, is removed to wherein cation impurity;
3) except anionic impurity:
Will be through step 2) liquid processed is by anion-exchange resin column, removes wherein anionic impurity, obtains rare lactic acid solution;
4) concentrated:
It is 80～90% that rare lactic acid solution is concentrated into to lactic acid content with evaporation equipment;
5) decolouring:
In the lactic acid solution after concentration, add discoloring agent to be decoloured, the add-on of discoloring agent is 0.05～8% of lactic acid solution quality after concentration, then carries out solid-liquid separation and remove discoloring agent, obtains finished product lactic acid.
Discoloring agent in described step 1) adopts one or more in diatomite, atlapulgite, gac;
In described step 1), solid-liquid separating equipment adopts one or more in filter press device, millipore filter, ultra filtration filter.
Described step 2) in, Zeo-karb adopts gel-type strongly acidic cation exchange resin or macroporous type storng-acid cation exchange resin, and crossing column flow rate is 0.5～6BV/h.
In described step 3), anionite-exchange resin adopts gel type strong basic anion exchange resin, macroporous type strongly basic anion exchange resin, gel type weakly basic anion exchange resin or macroporous type weak base anion-exchange resin, and crossing column flow rate is 0.5～6BV/h.
In described step 4), evaporation equipment adopts a kind of in double-effect evaporator or triple-effect evaporator.
Discoloring agent in described step 5) adopts one or more in diatomite, atlapulgite, gac;
In described step 5), described solid-liquid separating equipment adopts one or both in filter press device and millipore filter.
The present invention has following beneficial effect:
The present invention can realize that same batch of material repeatedly reclaims the purpose of cycling and reutilization, has farthest improved raw-material utilization ratio, has reduced the cost of silicon wafer stripping.Lactic acid in the useless lactic acid that energy efficient recovery silicon wafer stripping operation of the present invention produces, the rate of recovery is high, environmental pollution is little.Reclaim lactic acid and can continue on for silicon wafer stripping, or, for industries such as nickel plating, process hides and cleanings, can significantly reduce production costs, the very big pollution of simultaneously having avoided useless lactic acid to discharge causing to environment.
Further, the present invention adopts the measures such as the filtration of filter press device, essence filter and ultrafiltration to remove solid matter and organic macromolecule material in useless lactic acid, being concentrated into lactic acid content after spent ion exchange resin removal zwitterion impurity again is 80～90%, the lactic acid concn reclaimed is high, can continue on for silicon wafer stripping.
Embodiment
The method that reclaims lactic acid the useless lactic acid that the present invention produces from the silicon wafer stripping operation specifically comprises the following steps:
1) decolouring and separating solid substances
Add bleaching agent bleaching in useless lactic acid, the add-on of discoloring agent is 0.05～5% of useless lactic acid quality, then carries out solid-liquid separation and remove solids, obtains preliminary removal of impurities liquid.Wherein discoloring agent adopts one or more in diatomite, atlapulgite, gac; Solid-liquid separating equipment adopts one or more in filter press device, millipore filter, ultra filtration filter.
2) decationize impurity
The liquid of preliminary removal of impurities, by cation exchange resin column, is removed to wherein cation impurity.Wherein Zeo-karb adopts gel-type strongly acidic cation exchange resin or macroporous type storng-acid cation exchange resin, and crossing column flow rate is 0.5～6BV/h.
3) except anionic impurity
Will be through step 2) liquid processed is by anion-exchange resin column, removes wherein anionic impurity, obtains rare lactic acid solution.Wherein anionite-exchange resin adopts gel type strong basic anion exchange resin, macroporous type strongly basic anion exchange resin, gel type weakly basic anion exchange resin or macroporous type weak base anion-exchange resin, and crossing column flow rate is 0.5～6BV/h.
4) concentrated
By above-mentioned rare lactic acid solution, concentrated to be concentrated into lactic acid content with evaporation equipment be 80～90%.Wherein said evaporation equipment adopts double-effect evaporator or triple-effect evaporator.
5) decolouring
Add bleaching agent bleaching in the lactic acid solution after concentration, the add-on of discoloring agent is 0.05～8% of lactic acid solution quality after concentration, then carries out solid-liquid separation and remove discoloring agent, obtains finished product lactic acid.Wherein discoloring agent adopts one or more in diatomite, atlapulgite, gac; Solid-liquid separating equipment adopts one or both in filter press device and millipore filter.
Below provide several groups of preferred embodiments of the present invention:
Embodiment 1
1) stir decolouring to 0.05% the atlapulgite that adds useless lactic acid quality in useless lactic acid, adopt successively filter press device and ultra filtration filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 3BV/h by the gel-type strongly acidic cation exchange resin post, remove wherein cation impurity.
3) will be through step 2) liquid processed by the gel type strong basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 0.5BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with triple-effect evaporator is 81.7%.
5) to adding in the lactic acid solution after concentration 3.95% the diatomite that accounts for lactic acid solution quality after concentration and 0.05% atlapulgite to be decoloured, then carry out solid-liquid separation with the filter press device and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 81.8%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.002%, and this lactic acid can be used in silicon wafer stripping after tested.
Example 2
1) stir decolouring to 0.02% the activated carbon that adds useless lactic acid quality in useless lactic acid and 0.03% diatomite, adopt the filter press device to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 0.5BV/h by the gel-type strongly acidic cation exchange resin post, remove wherein cation impurity.
3) will be through step 2) liquid processed by macroporous type weak base anion-exchange resin post, removes wherein anionic impurity with the flow velocity of 6BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with double-effect evaporator is 85.2%.
5) to adding in the lactic acid solution after concentration 2.0% the gac that accounts for lactic acid solution quality after concentration and 2.0% atlapulgite to be decoloured, then carry out solid-liquid separation with filter press device and millipore filter successively and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 85.1%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.003%, and this lactic acid can be used in nickel plating after tested.
Example 3
1) stir decolouring to 5.0% the activated carbon that adds useless lactic acid quality in useless lactic acid, adopt successively filter press device, millipore filter and ultra filtration filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 6BV/h by the macroporous type strong acid cation exchange resin column, remove wherein cation impurity.
3) will be through step 2) liquid processed by the gel type weakly basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 3BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with triple-effect evaporator is 89.6%.
5) to adding in the lactic acid solution after concentration 0.05% the atlapulgite that accounts for lactic acid solution quality after concentration to be decoloured, then carry out solid-liquid separation with filter press device and millipore filter successively and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 89.5%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.002%, and this lactic acid can be used in the leather decalcification after tested.
Example 4
1) stir decolouring to 1.0% the diatomite that adds useless lactic acid quality in useless lactic acid and 1.5% atlapulgite, adopt successively filter press device and millipore filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 6BV/h by the gel-type strongly acidic cation exchange resin post, remove wherein cation impurity.
3) will be through step 2) liquid processed by macroporous type strongly basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 3BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with double-effect evaporator is 88.7%.
5) to adding in the lactic acid solution after concentration 0.03% the gac that accounts for lactic acid solution quality after concentration and 0.02% diatomite to be decoloured, then carry out solid-liquid separation with the filter press device and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 88.7%, and wherein molysite content (in Fe) is less than 0.002%, chloride content (in Cl) is less than 0.001%, and this lactic acid can be used as the scale remover raw material after tested.
Example 5
1) stir decolouring to 0.05% the activated carbon that adds useless lactic acid quality in useless lactic acid, adopt successively filter press device and ultra filtration filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 0.5BV/h by the macroporous type strong acid cation exchange resin column, remove wherein cation impurity.
3) will be through step 2) liquid processed by macroporous type strongly basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 6BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with double-effect evaporator is 85.1%.
5) to adding in the lactic acid solution after concentration 0.05% the gac that accounts for lactic acid solution quality after concentration and 4.0% atlapulgite to be decoloured, then carry out solid-liquid separation with filter press device and millipore filter successively and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 85.0%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.002%, and this lactic acid can be used in silicon wafer stripping after tested.
Example 6
1) stir decolouring to 2.5% the atlapulgite that adds useless lactic acid quality in useless lactic acid and 2.5% diatomite, adopt the filter press device to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 3BV/h by the macroporous type strong acid cation exchange resin column, remove wherein cation impurity.
3) will be through step 2) liquid processed by the gel type weakly basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 0.5BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with double-effect evaporator is 88.4%.
5) to adding in the lactic acid solution after concentration 8.0% the diatomite that accounts for lactic acid solution quality after concentration to be decoloured, then carry out solid-liquid separation with the filter press device and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 88.3%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.001%, and this lactic acid can be used in silicon wafer stripping after tested.
Example 7
1) stir decolouring to 1% the atlapulgite that adds useless lactic acid quality in useless lactic acid, 1% diatomite and 0.5% gac, adopt successively filter press device, millipore filter and ultra filtration filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 2BV/h by the gel-type strongly acidic cation exchange resin post, remove wherein cation impurity.
3) will be through step 2) liquid processed by macroporous type weak base anion-exchange resin post, removes wherein anionic impurity with the flow velocity of 2BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with triple-effect evaporator is 80.2%.
5) to adding in the lactic acid solution after concentration 1% the atlapulgite that accounts for lactic acid solution quality after concentration, 1% diatomite and 1% gac to be decoloured, then carry out solid-liquid separation with filter press device and millipore filter successively and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 80.1%, and wherein molysite content (in Fe) is less than 0.001%, chloride content (in Cl) is less than 0.002%, and this lactic acid can be used in the leather deliming after tested.
Example 8
1) stir decolouring to 5% the diatomite that adds useless lactic acid quality in useless lactic acid, adopt successively filter press device and millipore filter to carry out solid-liquid separation and remove solids, obtain preliminary removal of impurities liquid.
2) by the liquid of preliminary removal of impurities with the flow velocity of 6BV/h by the gel-type strongly acidic cation exchange resin post, remove wherein cation impurity.
3) will be through step 2) liquid processed by the gel type strong basic anion exchange resin post, removes wherein anionic impurity with the flow velocity of 3BV/h, obtains rare lactic acid solution.
4) above-mentioned rare lactic acid solution being concentrated into to lactic acid content with double-effect evaporator is 89.8%.
5) to adding in the lactic acid solution after concentration 4% the gac that accounts for lactic acid solution quality after concentration, 2% diatomite and 2% atlapulgite to be decoloured, then carry out solid-liquid separation with the filter press device and obtain finished product lactic acid.
Adopting the finished product lactic acid concn that aforesaid method obtains is 89.7%, and wherein molysite content (in Fe) is less than 0.002%, chloride content (in Cl) is less than 0.002%, and this lactic acid can be used in silicon wafer stripping after tested.
Claims (8)
1. a method that reclaims lactic acid from the useless lactic acid of silicon wafer stripping operation generation, is characterized in that, comprises the following steps:
1) decolouring and separating solid substances:
In useless lactic acid, add discoloring agent to be decoloured, the add-on of discoloring agent is 0.05～5% of useless lactic acid quality, then carries out solid-liquid separation and remove solids, obtains preliminary removal of impurities liquid;
2) decationize impurity:
The liquid of preliminary removal of impurities, by cation exchange resin column, is removed to wherein cation impurity;
3) except anionic impurity:
Will be through step 2) liquid processed is by anion-exchange resin column, removes wherein anionic impurity, obtains rare lactic acid solution;
4) concentrated:
It is 80～90% that rare lactic acid solution is concentrated into to lactic acid content with evaporation equipment;
5) decolouring:
In the lactic acid solution after concentration, add discoloring agent to be decoloured, the add-on of discoloring agent is 0.05～8% of lactic acid solution quality after concentration, then carries out solid-liquid separation and remove discoloring agent, obtains finished product lactic acid.
2. reclaim the method for lactic acid the useless lactic acid produced from the silicon wafer stripping operation according to claim 1, it is characterized in that: the discoloring agent in described step 1) adopts one or more in diatomite, atlapulgite, gac.
3. reclaim the method for lactic acid the useless lactic acid produced from the silicon wafer stripping operation according to claim 1 and 2, it is characterized in that: in described step 1), solid-liquid separating equipment adopts one or more in filter press device, millipore filter, ultra filtration filter.
4. reclaim the method for lactic acid the useless lactic acid produced from the silicon wafer stripping operation according to claim 1, it is characterized in that: described step 2), Zeo-karb adopts gel-type strongly acidic cation exchange resin or macroporous type storng-acid cation exchange resin, and crossing column flow rate is 0.5～6BV/h.
5. reclaim the method for lactic acid the useless lactic acid produced from the silicon wafer stripping operation according to claim 1, it is characterized in that: in described step 3), anionite-exchange resin adopts gel type strong basic anion exchange resin, macroporous type strongly basic anion exchange resin, gel type weakly basic anion exchange resin or macroporous type weak base anion-exchange resin, and crossing column flow rate is 0.5～6BV/h.
6. the method that reclaims lactic acid from the useless lactic acid that the silicon wafer stripping operation produces according to claim 1 is characterized in that: in described step 4), evaporation equipment adopts a kind of in double-effect evaporator or triple-effect evaporator.
7. reclaim the method for lactic acid the useless lactic acid produced from the silicon wafer stripping operation according to claim 1, it is characterized in that: the discoloring agent in described step 5) adopts one or more in diatomite, atlapulgite, gac.
8. according to reclaiming the method for lactic acid the described useless lactic acid produced from the silicon wafer stripping operation of claim 1 or 7, it is characterized in that: in described step 5), described solid-liquid separating equipment adopts one or both in filter press device and millipore filter.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072210A (en) * | 1992-08-21 | 1993-05-19 | 长沙食品添加剂厂 | The novel process of producing lactic acid by incrystallization |
| CN1427813A (en) * | 2000-03-07 | 2003-07-02 | 伊斯曼化学公司 | Process for recovery of organic acids from aqueous solutions |
| CN101880225A (en) * | 2010-06-04 | 2010-11-10 | 哈尔滨工业大学 | Method for extracting lactic acid from corn starch wastewater fermentation liquid by using anion exchange resin |
| CN102659564A (en) * | 2012-05-17 | 2012-09-12 | 安徽中粮生化格拉特乳酸有限公司 | Method for extracting lactic acid from wastewater generated in lactic acid production |
| CN202876519U (en) * | 2012-10-23 | 2013-04-17 | 镇江大成新能源有限公司 | Automatic degumming machine with lactic acid recovery function |
-
2013
- 2013-09-02 CN CN201310393353.8A patent/CN103450007B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072210A (en) * | 1992-08-21 | 1993-05-19 | 长沙食品添加剂厂 | The novel process of producing lactic acid by incrystallization |
| CN1427813A (en) * | 2000-03-07 | 2003-07-02 | 伊斯曼化学公司 | Process for recovery of organic acids from aqueous solutions |
| CN101880225A (en) * | 2010-06-04 | 2010-11-10 | 哈尔滨工业大学 | Method for extracting lactic acid from corn starch wastewater fermentation liquid by using anion exchange resin |
| CN102659564A (en) * | 2012-05-17 | 2012-09-12 | 安徽中粮生化格拉特乳酸有限公司 | Method for extracting lactic acid from wastewater generated in lactic acid production |
| CN202876519U (en) * | 2012-10-23 | 2013-04-17 | 镇江大成新能源有限公司 | Automatic degumming machine with lactic acid recovery function |
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