CN110272160A - Method for treating waste liquid and processing system in a kind of semiconductor preparing process - Google Patents

Method for treating waste liquid and processing system in a kind of semiconductor preparing process Download PDF

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Publication number
CN110272160A
CN110272160A CN201910564648.4A CN201910564648A CN110272160A CN 110272160 A CN110272160 A CN 110272160A CN 201910564648 A CN201910564648 A CN 201910564648A CN 110272160 A CN110272160 A CN 110272160A
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waste liquid
pickle liquor
liquid
pond
grinding
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尚菊红
张毅
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/20Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • C02F1/5245Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents using basic salts, e.g. of aluminium and iron
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/16Nitrogen compounds, e.g. ammonia
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)

Abstract

The present invention is suitable for environment protection field, provides method for treating waste liquid and processing system in a kind of semiconductor preparing process, the method comprise the steps that put into flocculant into grinding waste liquid, the grinding waste liquid that obtains that treated;Calcium hydroxide and heavy metal ion agent for capturing are put into pickle liquor, the pickle liquor that obtains that treated;Will treated grinding waste liquid pickle liquor mixes with treated, and carbon dioxide is passed through into mixed liquor;Nitric acid, ammonium hydroxide are sequentially added into treated mixed liquor again, is then concentrated by evaporation and urea-ammonium nitrate concentrate just can be obtained.Semiconductor method for treating waste liquid provided in an embodiment of the present invention, by separately being pre-processed to pickling section waste liquid and ground section waste liquid, it is mixed after having handled, take full advantage of the ammonium ion and nitrate ion in waste liquid, prepare urea-ammonium nitrate concentrate, while disposing waste liquid, using the active principle in waste liquid, economic benefit is improved.

Description

Method for treating waste liquid and processing system in a kind of semiconductor preparing process
Technical field
The invention belongs to method for treating waste liquid and processing systems in environment protection field more particularly to a kind of semiconductor preparing process System.
Background technique
A large amount of waste liquid can be generated in the preparation process flow of semiconductor, such as is needed in the etch process to semiconductor It carries out pickling and removes impurity, the oxidation film on surface etc. to generate largely containing acid waste liquid, in chemical mechanical milling tech The waste liquid largely containing lapping liquid, abrasive grains and ammonium hydroxide can equally be generated.
However, the waste liquid to each process section is all individually to handle, such as existing abrasive waste water is handled in existing technology Method be using ceramic membrane to grinding waste liquid be filtered, collect Recycling of waste liquid in abrasive grains, and will treated suspend Object concentration waste liquid that meet national standards is discharged, and such method for treating waste liquid is only intended merely to meet national discharge Standard, it is economically upper for it is unreasonable, the substance that can largely recycle directly is discharged.
As it can be seen that there is also serious problem of resource waste for existing semiconductor waste water processing method, being unfavorable for economy can Sustainable development.
Summary of the invention
The embodiment of the present invention is designed to provide method for treating waste liquid in a kind of semiconductor preparing process, it is intended to solve existing Some semiconductor waste water processing methods there is also serious problem of resource waste, the technology for being unfavorable for sustainable economic development asks Topic.
The embodiments of the present invention are implemented as follows, method for treating waste liquid in a kind of semiconductor preparing process, comprising:
The waste liquid generated to semiconductor grinding process section puts into flocculant, filters after sedimentation, the grinding waste liquid that obtains that treated;
Calcium hydroxide is put into the waste liquid generated to semiconductor acid cleaning process section, control pH is alkalinity, is settled after the reaction was completed simultaneously Filtering, the pickle liquor after obtaining single treatment;
Heavy metal ion agent for capturing is put into the pickle liquor of single treatment, is settled and is filtered after the reaction was completed, obtains secondary Treated pickle liquor;
By treated, grinding waste liquid is mixed with the pickle liquor after secondary treatment, carbon dioxide is passed through into waste liquid, and control PH is between 5 ~ 6, after the reaction was completed, settles and filters, the mixed waste liquor that obtains that treated;
To nitric acid is added in treated mixed waste liquor, heating removes carbon dioxide, adds ammonium hydroxide after cooling, be concentrated by evaporation To concentration liquid of ammonium nitrate.
The another object of the embodiment of the present invention is to provide liquid waste treatment system in a kind of semiconductor preparing process, including grinds It grinds liquid waste processing pond, pickle liquor single treatment pond, pickle liquor secondary treatment pond, mixing pit and is concentrated by evaporation pond, it is described It is connected between pickle liquor single treatment pond and pickle liquor secondary treatment pond by pipeline, the mixing pit and grinding waste liquid It is connected between processing pond, pickle liquor secondary treatment pond and evaporation and concentration pond by pipeline;
The grinding liquid waste processing pond, for handling grinding waste liquid by investment flocculant;
Pickle liquor single treatment pond, for carrying out single treatment to pickle liquor by investment calcium hydroxide;
Pickle liquor secondary treatment pond, for carrying out secondary place to pickle liquor by investment heavy metal ion agent for capturing Reason;
The mixing pit, for the grinding waste liquid after mixed processing and the pickle liquor after secondary treatment, and by being passed through two Carbonoxide handles mixed liquor;
The evaporation and concentration pond, for being concentrated by evaporation by successively putting into nitric acid and ammonium hydroxide into treated mixed liquor To concentration liquid of ammonium nitrate.
Method for treating waste liquid in a kind of semiconductor preparing process provided in an embodiment of the present invention, on the one hand by semiconductor Flocculant is put into the waste liquid that grinding workshop section generates, is filtered after sedimentation, obtains the grinding waste liquid containing ammonium ion concentration, it is another Aspect is precipitated the fluorine ion in waste liquid by putting into calcium hydroxide into the waste liquid of semiconductor acid cleaning process section, then puts into weight Metal ion capturing agent removes the heavy metal ion contained in waste liquid, obtains the grinding waste liquid containing nitrate ion concentration, will Treated grinding waste liquid and pickle liquor mixing, and further by waste liquid be passed through carbon dioxide remove excessive calcium from Nitric acid is added into waste liquid and heats up and removes carbon dioxide, is eventually adding ammonium hydroxide, removes excess of ammonia in evaporating concentration process for son Gas obtains more pure concentration liquid of ammonium nitrate, and by the above-mentioned processing to two kinds of waste liquids, finally having prepared can be used for preparing The intermediate products concentration liquid of ammonium nitrate of fertilizer, and the reactant being added in treatment process is that low-cost can directly buy Chemical products efficiently utilize the available ingredient in waste liquid, improve economic benefit, meet ring while disposing waste liquid While guaranteed request, the ideas of sustainable development has been also complied with.
Detailed description of the invention
Fig. 1 is liquid waste treatment system in a kind of semiconductor preparing process provided in an embodiment of the present invention;
Fig. 2 is liquid waste treatment system in another semiconductor preparing process provided in an embodiment of the present invention;
Fig. 3 is liquid waste treatment system in another semiconductor preparing process provided in an embodiment of the present invention.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
The embodiment of the present invention provides method for treating waste liquid in a kind of semiconductor preparing process, comprising:
The waste liquid generated to semiconductor grinding process section puts into flocculant, filters after sedimentation, the grinding waste liquid that obtains that treated;
Calcium hydroxide is put into the waste liquid generated to semiconductor acid cleaning process section, control pH is alkalinity, is settled after the reaction was completed simultaneously Filtering, the pickle liquor after obtaining single treatment;
Heavy metal ion agent for capturing is put into the pickle liquor of single treatment, is settled and is filtered after the reaction was completed, obtains secondary Treated pickle liquor;
By treated, grinding waste liquid is mixed with the pickle liquor after secondary treatment, carbon dioxide is passed through into waste liquid, and control PH is between 4.5 ~ 6, after the reaction was completed, settles and filters, the mixed waste liquor that obtains that treated;
To nitric acid is added in treated mixed waste liquor, heating removes carbon dioxide, adds ammonium hydroxide after cooling, be concentrated by evaporation To concentration liquid of ammonium nitrate.
In embodiments of the present invention, the waste liquid that semiconductor grinding process section generates mainly includes lapping liquid, abrasive grains, In contain a large amount of ammonium ion, since the primary pollution source in this segment process waste water is abrasive grains i.e. suspended matter, existing skill Most of art is the abrasive grains in removing waste liquid, so that after the content of suspended matter meets national regulation, with regard to direct emission.Example Such as, waste liquid is filtered to remove abrasive grains using ceramic membrane.And the present invention removes abrasive grains by the way that flocculant is added Afterwards, it makes full use of ammonium ion present in waste liquid as the raw material for preparing fertiliser intermediate, improves economic benefit.
In embodiments of the present invention, the waste liquid that semiconductor acid cleaning process section generates mainly includes the acid solutions such as hydrofluoric acid, nitric acid And heavy metal ion, the prior art are usually to add lye after removing hydrofluoric acid and the heavy metal ion in waste liquid Acid-base neutralization is carried out, so that the pH of waste liquid reaches permission discharge standard.And the present invention is by removing hydrofluoric acid, that is, fluorine in solution After ion and heavy metal ion, using prepare in nitrate ion, with grinding technics present in waste liquid containing ammonium root from The waste water mixing of son further can prepare fertilizer by ammonium nitrate to prepare ammonium nitrate.
In embodiments of the present invention, by the way that calcium hydroxide is added into solution, introducing calcium ion can be effectively and in solution Fluorine ion combine generate calcium fluoride precipitate, to remove the calcirm-fluoride in solution, it is contemplated that the dissolution of calcium hydroxide in water Degree is not high, and the present invention is preferably added to saturation lime stone solution i.e. calcium hydroxide solution, compared to solid limestone particle is added, instead Should more rapidly, fluoride ion removing effect is more preferable.
In embodiments of the present invention, by be added heavy metal ion agent for capturing can effectively with the heavy metal in solution Complex reaction occurs for ion (mainly copper ion), so that the heavy metal ion in solution is removed, the heavy metal of commercial type Ion capturing agent has very much, and counterweight metal ion capturing agent does not do specific restriction to the present invention.
In embodiments of the present invention, due to ammonium nitrate during preparing fertilizer to the more demanding of purity, and removing Go the calcium ion introduced during fluorine ion larger to the impurities affect of ammonium nitrate, for this purpose, we into mixed liquor by leading to Enter carbon dioxide, so that the calcium ion in mixed liquor first precipitates, further, by the way that a small amount of nitric acid is added and heats to remove Remove the carbonate introduced, it is preferred that the temperature of heating is controlled, and a small amount of ammonium hydroxide progress is further added at 30 °C ~ 60 °C It neutralizes, removes excess of ammonia while being concentrated by evaporation, finally obtain the ammonium nitrate solution of purity is high, it is preferred that be concentrated by evaporation During temperature control at 25 °C ~ 50 °C.
In embodiments of the present invention, it is contemplated that " put into the waste liquid generated to semiconductor acid cleaning process section in following step Calcium hydroxide, control pH is alkalinity, settles and filters after the reaction was completed " " heavy metal is put into the pickle liquor of single treatment Ion capturing agent is settled after the reaction was completed and is filtered, the pickle liquor after obtaining secondary treatment " and " will treated grinding Waste liquid is mixed with the pickle liquor after secondary treatment, and carbon dioxide is passed through into waste liquid, and controls pH between 5 ~ 6, has been reacted Cheng Hou is settled and is filtered ", it is all by way of generating precipitating/complex compound to remove the respective substance in solution, and it is naturally heavy That drops is relatively inefficient, can be by flocculant being added into solution to improve sewage treating efficiency, it is preferred that the flocculation Organic polymer coargulator is selected in agent.
In embodiments of the present invention, it is contemplated that during Removal of F- ion, to guarantee that fluorine ion completely removes, preferably In pickle liquor processing pond inlet using the fluorinion concentration in fluorine ion measuring instrument detection pickle liquor, and combine at waste liquid The volume in reason pond determines the fluorine ion total amount contained in waste liquid, to determine the calcium hydroxide launched according to fluorine ion total amount, makes The micro- excess of amount of calcium hydroxide is obtained, to guarantee optimal anion removal effect.
In embodiments of the present invention, the outlet of liquid waste processing pond being exported and ground in pickle liquor processing pond, nitre state is respectively set Nitrate ion concentration and place in Nitrogen ion concentration measuring apparatus and ammonium ion ammonia nitrogen detector test treated pickle liquor The ammonium ion concentration in grinding waste liquid after reason, can control according to the nitrate ion concentration and ammonium ion concentration Mixed volume ratio of the waste liquid with pickle liquor when mixing is ground, so that mixed nitrate ion concentration and ammonium ion Concentration maintains the level of relative equilibrium.
As shown in Figure 1, details are as follows the present invention also provides liquid waste treatment system in a kind of semiconductor preparing process.
In embodiments of the present invention, liquid waste treatment system includes grinding liquid waste processing pond in the semiconductor preparing process 101, pickle liquor single treatment pond 102, pickle liquor secondary treatment pond 103, mixing pit 104 and evaporation and concentration pond 105, institute It states and is connected between pickle liquor single treatment pond 102 and pickle liquor secondary treatment pond 103 by pipeline, the mixing pit It is connected between 104 and grinding liquid waste processing pond 101, pickle liquor secondary treatment pond 103 and evaporation and concentration pond 105 by pipeline It is logical.
The grinding liquid waste processing pond 101, for handling grinding waste liquid by investment flocculant.
In embodiments of the present invention, the waste liquid that semiconductor grinding process section generates mainly includes lapping liquid, abrasive grains, is gone back Ammonium ion present in waste liquid is made full use of after flocculant removing abrasive grains are added containing a large amount of ammonium ion As the raw material for preparing fertiliser intermediate, economic benefit is improved.
Pickle liquor single treatment pond 102, for once being located to pickle liquor by investment calcium hydroxide Reason.
In embodiments of the present invention, the waste liquid that semiconductor acid cleaning process section generates mainly includes the acid solutions such as hydrofluoric acid, nitric acid And heavy metal ion, fluorine ion present in waste liquid can be effectively removed by the way that calcium hydroxide is added.
Pickle liquor secondary treatment pond 103, for being carried out to pickle liquor by investment heavy metal ion agent for capturing Secondary treatment.
In embodiments of the present invention, by be added heavy metal ion agent for capturing can effectively with the heavy metal in solution Complex reaction occurs for ion (mainly copper ion), to remove the heavy metal ion in solution.
The mixing pit 104 for the grinding waste liquid after mixed processing and the pickle liquor after secondary treatment, and passes through It is passed through carbon dioxide, mixed liquor is handled.
It is in embodiments of the present invention, larger to the impurities affect for the ammonium nitrate finally prepared due to introducing calcium ion, Therefore it needs to remove calcium ion, it, can be by calcium ions precipitate by being passed through carbon dioxide into mixed liquor.
The evaporation and concentration pond 105, for by successively put into treated mixed liquor nitric acid and, be concentrated by evaporation Obtain concentration liquid of ammonium nitrate.
In embodiments of the present invention, further solution can be purified by the way that nitric acid and ammonium hydroxide are added again, is steamed The concentration liquid of ammonium nitrate of available purity is high, the fertilizer quality prepared are more preferable after hair concentration.
As another embodiment of the invention, as shown in Fig. 2, liquid waste treatment system in a kind of semiconductor preparing process, Difference with liquid waste treatment system in a kind of semiconductor preparing process shown in fig. 1 is:
It is equipped with ammonium ion ammonia nitrogen detector 201 in 101 exit of grinding liquid waste processing pond, treated grinds for measuring Ammonium ion concentration in waste liquid.
It is equipped with fluorine ion measuring instrument 202 in 102 inlet of pickle liquor single treatment pond, to measure semiconductor acid Wash the fluorinion concentration in the waste liquid of process section generation.
It is equipped with nitrate nitrogen ion concentration measurement instrument 203 in 103 exit of pickle liquor secondary treatment pond, for measuring The nitrate ion concentration in pickle liquor after secondary treatment.
In embodiments of the present invention, it is contemplated that during Removal of F- ion, to guarantee that fluorine ion completely removes, preferably In pickle liquor processing pond inlet using the fluorinion concentration in fluorine ion measuring instrument detection pickle liquor, and combine at waste liquid The volume in reason pond determines the fluorine ion total amount contained in waste liquid, to determine the calcium hydroxide launched according to fluorine ion total amount, makes The micro- excess of amount of calcium hydroxide is obtained, to guarantee optimal anion removal effect.
In embodiments of the present invention, the outlet of liquid waste processing pond being exported and ground in pickle liquor processing pond, nitre state is respectively set Nitrate ion concentration and place in Nitrogen ion concentration measuring apparatus and ammonium ion ammonia nitrogen detector test treated pickle liquor The ammonium ion concentration in grinding waste liquid after reason, can control according to the nitrate ion concentration and ammonium ion concentration Mixed volume ratio of the waste liquid with pickle liquor when mixing is ground, so that mixed nitrate ion concentration and ammonium ion Concentration maintains the level of relative equilibrium.
As another embodiment of the invention, as shown in figure 3, liquid waste treatment system in a kind of semiconductor preparing process, With Fig. 2 shows a kind of semiconductor preparing process in the difference of liquid waste treatment system be:
On the pipeline that the mixing pit 104 is connected with grinding liquid waste processing pond 101, pickle liquor secondary treatment pond 103 respectively Equipped with flow control valve 301 and 302, after according to the ammonium ion concentration and nitrate ion concentration control processing Grinding waste liquid and secondary treatment after pickle liquor mixing ratio.
In order to keep above scheme more specific, following examples are provided.
Embodiment 1:
8 tons of waste liquid uniform effluents that semiconductor grinding process section is generated extremely are ground in liquid waste processing pond, wherein semiconductor grinding The waste liquid that process section generates is to the alkaline slurries (manufacturer: Hitachi's chemical conversion industry (Dongguan) Co., Ltd using market sale Series: HS-8005) semiconductor is ground so as to be generated during element surface is smooth;
Polyacrylamide is put into according to the dosage of 5ppm into grinding liquid waste processing pond, reacts and settles 1 hour, removes precipitating Supernatant is emitted into mixing pit by object;
5 tons of waste liquid uniform effluents that semiconductor acid cleaning process section is generated are into pickle liquor single treatment pond, wherein semiconductor The waste liquid that acid cleaning process section generates is to compound mixed acid obtained according to the volume ratio of 2:1 using nitric acid and hydrofluoric acid half-and-half to lead Body surface face generate during cleaning impurity and oxidation film;
Solid limestone particle is put into pickle liquor single treatment pond and adjusts pH to 7.5, is reacted and is settled 4 hours, removes Supernatant is emitted into pickle liquor secondary treatment pond by sediment;
Into pickle liquor secondary treatment pond according to the heavy metal ion agent for capturing (factory of the dosage investment commercial type of 200ppm Quotient: Guangzhou indigo plant Feng Environmental Protection Technology Co., Ltd), it reacts and settles 4 hours, remove sediment, supernatant is emitted into mixing pit In;
When treated grinding waste liquid and treated pickle liquor mixes in mixing pit after, titanium dioxide is passed through into mixing pit Carbon, adjusting pH is 6, reacts and settles 2 hours, removes sediment, and supernatant is emitted into and is concentrated by evaporation in pond;
The dust technology that investment concentration is 30% into evaporation and concentration pond is 4.5 to pH, keeps the temperature 1 hour under 30 °C of environment to remove Carbon dioxide adds the ammonium hydroxide that concentration is 20% and adjusts pH to 6.5, is then concentrated by evaporation under 25 °C of environment after cooling Obtain about 10 tons of concentration liquid of ammonium nitrate that mass fraction is 12%.
Embodiment 2:
8 tons of waste liquid uniform effluents that semiconductor grinding process section is generated extremely are ground in liquid waste processing pond, wherein semiconductor grinding The waste liquid that process section generates is to the alkaline slurries (manufacturer: Hitachi's chemical conversion industry (Dongguan) Co., Ltd using market sale Series: HS-8005) semiconductor is ground so as to be generated during element surface is smooth;
Diallyl dimethyl ammoniumchloride is put into according to the dosage of 8ppm into grinding liquid waste processing pond, react and settles 1 is small When, sediment is removed, supernatant is emitted into mixing pit;
5 tons of waste liquid uniform effluents that semiconductor acid cleaning process section is generated into pickle liquor single treatment pond, wherein semiconductor The waste liquid that acid cleaning process section generates is to compound mixed acid obtained according to the volume ratio of 1:1 using nitric acid and hydrofluoric acid half-and-half to lead Body surface face generate during cleaning impurity and oxidation film;
Lime stone solution is put into pickle liquor single treatment pond and adjusts pH to 8, and puts into polydiene according to the dosage of 2ppm Diallyidimethylammonium chloride is reacted and is settled 1 hour, removes sediment, supernatant is emitted into pickle liquor secondary treatment pond In;
Into pickle liquor secondary treatment pond according to the heavy metal ion agent for capturing (factory of the dosage investment commercial type of 250ppm Quotient: Guangzhou indigo plant Feng Environmental Protection Technology Co., Ltd), it reacts and settles 4 hours, remove sediment, supernatant is emitted into mixing pit In;
When treated grinding waste liquid and treated pickle liquor mixes in mixing pit after, titanium dioxide is passed through into mixing pit Carbon, adjusting pH is 5.5, reacts and settles 2 hours, removes sediment, and supernatant is emitted into and is concentrated by evaporation in pond;
The dust technology that investment concentration is 25% into evaporation and concentration pond is 4.8 to pH, keeps the temperature 1 hour under 45 °C of environment to remove Carbon dioxide adds the ammonium hydroxide that concentration is 22% and adjusts pH to 6.8, is then concentrated by evaporation under 35 °C of environment after cooling Obtain about 9 tons of concentration liquid of ammonium nitrate that mass fraction is 10%.
Embodiment 3:
8 tons of waste liquid uniform effluents that semiconductor grinding process section is generated extremely are ground in liquid waste processing pond, wherein semiconductor grinding The waste liquid that process section generates is to the alkaline slurries (manufacturer: Hitachi's chemical conversion industry (Dongguan) Co., Ltd using market sale Series: HS-8005) semiconductor is ground so as to be generated during element surface is smooth;
Polyacrylamide is put into according to the dosage of 8ppm into grinding liquid waste processing pond, reacts and settles 1 hour, removes precipitating Supernatant is emitted into mixing pit by object;
5 tons of waste liquid uniform effluents that semiconductor acid cleaning process section is generated are into pickle liquor single treatment pond, wherein semiconductor The waste liquid that acid cleaning process section generates is to compound mixed acid obtained according to the volume ratio of 1:2 using nitric acid and hydrofluoric acid half-and-half to lead Body surface face carry out cleaning impurity and oxidation film during generate, mainly contain the heavy metals such as nitric acid, hydrofluoric acid and copper, chromium from Son;
Into pickle liquor single treatment pond, investment saturation lime stone solution adjusts pH to 8.5, reacts and settles 4 hours, removes Supernatant is emitted into pickle liquor secondary treatment pond by sediment;
Into pickle liquor secondary treatment pond according to the heavy metal ion agent for capturing (factory of the dosage investment commercial type of 300ppm Quotient: Guangzhou indigo plant Feng Environmental Protection Technology Co., Ltd), polyacrylamide then is put into according to the dosage of 2ppm, reacts and to settle 1 small When, sediment is removed, supernatant is emitted into mixing pit;
When treated grinding waste liquid and treated pickle liquor mixes in mixing pit after, titanium dioxide is passed through into mixing pit Carbon, adjusting pH is 5, reacts and settles 2 hours, removes sediment, and supernatant is emitted into and is concentrated by evaporation in pond;
The dust technology that investment concentration is 20% into evaporation and concentration pond is to keep the temperature 1 hour under 5,60 °C of environment to remove dioxy to pH Change carbon, the ammonium hydroxide that concentration is 25% is added after cooling and adjusts pH to 7.2, being then concentrated by evaporation under 50 °C of environment can be obtained Mass fraction is about 8 tons of concentration liquid of ammonium nitrate of 10%.
It, can be by semiconductor grinding section waste water and semiconductor pickling section wastewater treatment at quality by above-mentioned processing method Concentration liquid of ammonium nitrate of the score 10% ~ 12%, may further prepare high efficiency liquid nitrogenous fertilizer, have very high economic benefit.It presses It is calculated according to 100 ton/days of total wastewater treatment capacities, concentration liquid of ammonium nitrate is up to 65 ~ 85 ton/days, the generally nitrogen in waste liquid Utilization rate is 90% or more.
In embodiment provided by the invention, on the one hand by putting into flocculant in the waste liquid that generates to semiconductor grinding workshop section Remove the abrasive grains that contain in waste liquid, filtered after sedimentation, obtain the grinding waste liquid containing ammonium ion, on the other hand pass through to Calcium hydroxide is put into the waste liquid of semiconductor acid cleaning process section, is first precipitated the fluorine ion in waste liquid, then put into heavy metal ion Agent for capturing further removes the heavy metal ion contained in waste liquid, obtains the grinding waste liquid containing nitrate ion concentration, will locate Grinding waste liquid and pickle liquor mixing after reason, obtain the mixing containing nitrate ion, ammonium ion and a small amount of calcium ion Liquid, and further by being passed through carbon dioxide to waste liquid to remove excessive calcium ion, and nitric acid is added into waste liquid and heats up Carbon dioxide is removed, ammonium hydroxide is eventually adding, excessive ammonia is removed in evaporating concentration process, while obtaining the nitric acid of purity is high Ammonium concentrate has finally prepared the intermediate products ammonium nitrate that can be used for preparing fertilizer by the above-mentioned processing to two kinds of waste liquids Concentrate, and the reactant being added in treatment process is the low-cost chemical products that can directly buy, and is being disposed waste liquid While, the available ingredient in waste liquid is efficiently utilized, economic benefit is improved, while meeting environmental requirement, is also complied with The ideas of sustainable development.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously Limitations on the scope of the patent of the present invention therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to guarantor of the invention Protect range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all in essence of the invention Made any modifications, equivalent replacements, and improvements etc., should all be included in the protection scope of the present invention within mind and principle.

Claims (10)

1. method for treating waste liquid in a kind of semiconductor preparing process characterized by comprising
The waste liquid generated to semiconductor grinding process section puts into flocculant, filters after sedimentation, the grinding waste liquid that obtains that treated;
Calcium hydroxide is put into the waste liquid generated to semiconductor acid cleaning process section, control pH is alkalinity, is settled after the reaction was completed simultaneously Filtering, the pickle liquor after obtaining single treatment;
Heavy metal ion agent for capturing is put into the pickle liquor of single treatment, is settled and is filtered after the reaction was completed, obtains secondary Treated pickle liquor;
By treated, grinding waste liquid is mixed with the pickle liquor after secondary treatment, carbon dioxide is passed through into waste liquid, and control PH is between 5 ~ 6, after the reaction was completed, settles and filters, the mixed waste liquor that obtains that treated;
To nitric acid is added in treated mixed waste liquor, heating removes carbon dioxide, adds ammonium hydroxide after cooling, be concentrated by evaporation To concentration liquid of ammonium nitrate.
2. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that the flocculant choosing Use organic polymer coargulator.
3. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that the calcium hydroxide Select saturation lime stone solution.
4. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that described to partly leading It further include using described in the measurement of fluorine ion measuring instrument before the step of putting into calcium hydroxide in the waste liquid that body acid cleaning process section generates The fluorinion concentration in waste liquid that semiconductor acid cleaning process section generates, and based on fluorinion concentration and waste liquid volume into waste liquid Put into the calcium hydroxide of amount corresponding with fluorine ion total amount.
5. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that will be handled described It further include being surveyed using ammonium ion ammonia nitrogen detector before the step of grinding waste liquid afterwards is mixed with the pickle liquor after secondary treatment Ammonium ion concentration in fixed treated grinding waste liquid, the acid after utilizing the measurement secondary treatment of nitrate nitrogen ion concentration measurement instrument The nitrate ion concentration in waste liquid is washed, and treated based on the ammonium ion concentration and nitrate ion concentration control Grind mixing ratio of the waste liquid with the pickle liquor after secondary treatment when mixing.
6. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that the heating removes In the step of carbon dioxide, warming temperature is controlled at 30 °C ~ 60 °C.
7. method for treating waste liquid in semiconductor preparing process according to claim 1, which is characterized in that the evaporation and concentration In the step of obtaining concentration liquid of ammonium nitrate, temperature is controlled at 25 °C ~ 50 °C.
8. liquid waste treatment system in a kind of semiconductor preparing process, which is characterized in that including grinding liquid waste processing pond, pickle liquor Single treatment pond, pickle liquor secondary treatment pond, mixing pit and evaporation and concentration pond, pickle liquor single treatment pond and acid It washes between waste liquid secondary treatment pond and is connected by pipeline, the mixing pit and grinding liquid waste processing pond, the secondary place of pickle liquor It is connected between reason pond and evaporation and concentration pond by pipeline;
The grinding liquid waste processing pond, for handling grinding waste liquid by investment flocculant;
Pickle liquor single treatment pond, for carrying out single treatment to pickle liquor by investment calcium hydroxide;
Pickle liquor secondary treatment pond, for carrying out secondary place to pickle liquor by investment heavy metal ion agent for capturing Reason;
The mixing pit, for the grinding waste liquid after mixed processing and the pickle liquor after secondary treatment, and by being passed through two Carbonoxide handles mixed liquor;
The evaporation and concentration pond, for being concentrated by evaporation by successively putting into nitric acid and ammonium hydroxide into treated mixed liquor To concentration liquid of ammonium nitrate.
9. liquid waste treatment system in semiconductor preparing process according to claim 8, which is characterized in that the grinding waste liquid Processing pond exit is equipped with ammonium ion ammonia nitrogen detector, and the ammonium ion concentration in waste liquid, institute are ground for measure that treated Pickle liquor single treatment pond inlet is stated equipped with fluorine ion measuring instrument, to measure the waste liquid of semiconductor acid cleaning process section generation In fluorinion concentration, pickle liquor secondary treatment pond exit be equipped with nitrate nitrogen ion concentration measurement instrument, for measuring The nitrate ion concentration in pickle liquor after secondary treatment.
10. liquid waste treatment system in semiconductor preparing process according to claim 9, which is characterized in that the mixing pit It is respectively equipped with flow control valve on the pipeline being connected with grinding liquid waste processing pond, pickle liquor secondary treatment pond, is used for basis The ammonium ion concentration and nitrate ion concentration control treated grinding waste liquid and secondary treatment after pickle liquor Mixing ratio.
CN201910564648.4A 2019-06-27 2019-06-27 Method for treating waste liquid and processing system in a kind of semiconductor preparing process Withdrawn CN110272160A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115057552A (en) * 2022-06-23 2022-09-16 先导薄膜材料有限公司 Concentration method of low-concentration ammonium nitrate wastewater

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115057552A (en) * 2022-06-23 2022-09-16 先导薄膜材料有限公司 Concentration method of low-concentration ammonium nitrate wastewater

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