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 PDFInfo
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
- C02F1/5245—Treatment 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy 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
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.
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Cited By (1)
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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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Cited By (1)
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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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