CN105112017A - Environment-friendly snow melting agent prepared from alkaline residues and preparation method therefor - Google Patents
Environment-friendly snow melting agent prepared from alkaline residues and preparation method therefor Download PDFInfo
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Abstract
The present invention relates to an environment-friendly snow melting agent prepared from alkaline residues and a preparation method therefor. The environment-friendly snow melting agent comprises a product obtained by a reaction which takes the alkaline residues and acid as raw materials, and preferably comprises one or more of urea, sodium nitrite and magnesium acetate. The preparation method for the product comprises: under a condition of stirring, adding the acid to a reaction tank with the alkaline residues and performing reaction; adjusting the pH value of a reaction system to 7-8 by use of the alkali residues or the acid so as to obtain suspended reaction liquor, and filtering the suspended reaction liquor to obtain the product. The present invention firstly discloses the environment-friendly snow melting agent which is prepared by taking the alkali residues and the acid as raw materials, solves the alkali residue treatment problem, improves the economic value of the alkali residues, and obtains a byproduct carbon dioxide. The method disclosed by the invention is simple and easy to implement. The environment-friendly snow melting agent prepared by the method is good in effect and, green and environmentally friendly; and the production cost of the snow melting agent is obviously reduced.
Description
Technical field
The invention belongs to comprehensive utilization and the chemical production technical field of chemical sludge, particularly relate to a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare and preparation method thereof.
Background technology
Snow Agent (road freezes preventing agent) is mainly used in road, airport, harbour, avenue cleaning snow in winter and road anti-freeze.The Snow Agent of domestic and international use generally has two large classes: a class take acetate as the Snow Agent of main component, and such Snow Agent snow melt is effective, has nothing corrosion-damaged, but its price is high, is generally used for the important places such as airport.Another kind of is the Snow Agent that is main component with " villaumite ", as sodium-chlor, calcium chloride, magnesium chloride, Repone K etc., so-called " change cryosel ".Domestic main environment-friendly snowmelt agent has calcium chloride, inhibiter, slipproofing agent etc., through pulverizing, stirring, mixes i.e. obtained novel environment friendly Snow Agent.But the synthesis of the calcium chloride of routine adopts Wingdale to be raw material, raw material and tooling cost high.Snow Agent disclosed in Chinese patent application CN200910011620.4 is prepared by calcium source by shell, Ovum crusta Gallus domesticus, but shell, eggshell not easily collecting, and need to carry out pulverizing and preprocessing, add cost.
Alkaline residue is the waste residue discharged in solvay soda process alkali producing process, and its main component is calcium carbonate, calcium hydroxide.Due to solvay soda process soda manufacture technique, often produce the alkaline residue that 1 ton of soda ash outwards will discharge 0.3-0.4 ton.Domestic ammonia alkali factory takes the mode process alkaline residue that nature is stacked or directly row is extra large mostly.The problem caused is as follows: (1) occupies a large amount of land resources, and objectionable constituent are wherein the water and soil that permeates the ground through the erosion of Weathering And Leaching, rainwash, pollutes; The original structure of spoiled soil, finally develops into saltings simultaneously.(2) alkaline residue row Hai Ze causes marine ecology balance destroyed, harm aquaculture, and may jeopardize navigation channel after deposition.Therefore, the problem of alkaline residue governs further developing of soda ash enterprise always, is a large technical barrier of ammonia alkali factory.
In view of this, special proposition the present invention.
Summary of the invention
The object of the invention is to overcome the problem that alkaline residue is difficult to utilize, a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare and preparation method thereof is provided.Main composition-calcium carbonate, calcium hydroxide in alkaline residue, can generate calcium salt with acid-respons.And compare, alkaline residue has following advantage: output is large, compares shell, eggshell is easily collected; Granularity is little, compares the process that Wingdale, shell and eggshell decrease pulverizing, cost-saving; Definite ingredients, reacts controlled.
: a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare that comprising by alkaline residue and acid is the product that raw material carries out reacting for realizing the object of the invention the technical solution adopted in the present invention.
Wherein, described acid is one or more in hydrochloric acid, acetic acid, waste hydrochloric acid, wood vinegar, sulfuric acid etc.; Preferably, described acid is hydrochloric acid and acetic acid.
Usually, the content of alkaline residue neutral and alkali calcium salt of the present invention is not less than 70%; Preferred described alkaline calcium salt comprises one or more in calcium carbonate, calcium sulfate, calcium chloride etc.
Usually, also Ca (OH) is contained in alkaline residue of the present invention
2, content is about about 10%.
Such as, alkaline residue of the present invention is the waste residue discharged in solvay soda process alkali producing process.
Described is the product that raw material carries out reacting by alkaline residue and acid, the preparation method of this product comprises: under the condition stirred, acid is joined in the retort that alkaline residue is housed and reacts, then reaction system pH to 7-8 is regulated with described alkaline residue or described acid, the reaction solution of state must be suspended, filter, obtain liquid product; Or further by described liquid product through evaporation, dry, obtain solid product.
Usually, described solid product water content≤15%.
Above-mentioned is that raw material carries out in the preparation method of the product reacted by alkaline residue and acid:
Described acid is hydrochloric acid and/or acetic acid; Be preferably hydrochloric acid and acetic acid.
Usually, the time of carrying out reacting in described retort is generally 5-6 hour.
Preferably, described in be filtered into vacuum filtration, preferred vacuum tightness is 1-20kPa.
Further, desolventing technology can be carried out to described liquid product.Preferred decoloration treatment method is charcoal absorption decolouring.
Byproduct carbonic acid gas can be obtained by reclaiming the carbonic acid gas (such as adopting siccative) produced in described reaction.Carbonic acid gas can be applied in the technique of ammonia-soda process soda ash and go.
Further, the hydrogen chloride gas that can also volatilize in absorption reaction process.
Above-mentioned liquid product (comprise decolouring or nondiscoloration) is concentrated or can directly as the environment protection snow-dissolved agent of liquid state after concentrated.
Or by above-mentioned liquid product (comprise decolouring or nondiscoloration) obtained solid product further after evaporation, drying, described solid product is used as environment protection snow-dissolved agent.
For improving snow melt further, changing ice effect, described environment protection snow-dissolved agent also comprises one or more in urea, Sodium Nitrite, acetate (such as magnesium acetate), sodium-chlor, calcium chloride, magnesium chloride, Repone K etc.
Particularly, described environment protection snow-dissolved agent, comprising by alkaline residue and hydrochloric acid and/or acetic acid is the product that raw material carries out reacting; Preferably, one or more in urea, Sodium Nitrite, magnesium acetate are also comprised.Usually, by each component routinely technology mix and can obtain.
More specifically, described environment protection snow-dissolved agent, with parts by weight, comprise by alkaline residue and hydrochloric acid be raw material carry out reacting solid product 75-95 part, urea 5-15 part, Sodium Nitrite 0-10 part.
Or described environment protection snow-dissolved agent, with parts by weight, comprise by alkaline residue and acetic acid be raw material carry out reacting solid product 10-50 part, magnesium acetate 50-90 part.
The present invention is surprised to find that, when containing with above-mentioned alkaline residue and hydrochloric acid and acetic acid for raw material carries out the environment protection snow-dissolved agent of the product reacted, its deicing or snow melting effect is better.
Particularly, a kind of environment protection snow-dissolved agent, with parts by weight, comprise by alkaline residue and hydrochloric acid and acetic acid be raw material carry out reacting solid product 50-80 part, urea 6-9 part, Sodium Nitrite 3-4.5 part, magnesium acetate 9-36 part.
Weight part of the present invention can be the weight unit well known in the art such as g, kg, also can be its multiple, as 1/10,1/100,10 times, 100 times etc.
Environment protection snow-dissolved agent of the present invention can be solid-state or liquid.
Beneficial effect of the present invention is:
The present invention proposes, by adopting alkaline residue to prepare environment protection snow-dissolved agent with acid for raw material, not only effectively to make use of the calcium ion in alkaline residue, also make the existence of chlorion become favorable factor first.Both solve a difficult problem for alkaline residue process, also improved alkaline residue economic worth, obtain byproduct carbonic acid gas simultaneously.If utilize alkaline residue and spent acid to react prepare environment protection snow-dissolved agent, the economic worth of spent acid can also be improved.The inventive method is simple and easy to do, and secondary pollution is few, and obtained environment protection snow-dissolved agent had both had good snow melt, changed ice effect, also had the advantage of environmental protection; Compared with traditional Snow Agent sodium-chlor, greatly reduce the corrosive nature to metal ion and road surface, and significantly reduce the production cost of Snow Agent.In addition, because environment protection snow-dissolved agent of the present invention contains calcium salt and urea etc., as the fertilizer of roadside plant, can also achieve many things at one stroke.
Accompanying drawing explanation
The XRD figure spectrum of Fig. 1 environment protection snow-dissolved agent obtained by embodiment 1;
The XRD figure spectrum of Fig. 2 environment protection snow-dissolved agent obtained by embodiment 5;
Fig. 3 is the corrosion condition figure of the drawing pin of experimental example 5;
Wherein, in Fig. 1 and Fig. 2, X-coordinate " 2-Theta-Scale " expression " 2 θ angle "; Ordinate zou " Intensity " expression " peak is strong ";
The environment protection snow-dissolved agent process that in Fig. 3, I, II, III represent distilled water process respectively, the embodiment 1 of 20% (wt) obtains, the sodium-chlor process of 20% (wt).
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.As indicated without special, the raw materials used alkaline residue of following examples originates from Tangshan three You Jian factory.
Embodiment 1
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprising by alkaline residue and hydrochloric acid is the solid product that raw material carries out reacting.
The present embodiment provides the preparation method of this solid product simultaneously, under being included in the condition of stirring, slowly being joined in the retort that alkaline residue has been housed by concentrated hydrochloric acid and reacts, and after reaction carries out 5-6 hour, detects pH; To regulate in retort pH when 7-8 with alkaline residue, concentrated hydrochloric acid, stopped reaction, must be suspended the reaction solution of state, then carries out vacuum filtration, vacuum tightness 20kPa, evaporation, dry, obtained solid product.This solid product directly can be used as environment protection snow-dissolved agent.
The byproduct carbonic acid gas of reaction is reclaimed in reaction process.
Its reaction formula is:
CaCO
3+2HCl＝CaCl
2+H
2O+CO
2↑
Ca(OH)
2+2HCl＝CaCl
2+2H
2O
The present embodiment Raw charging capacity and product amount see the following form 1.
Table 1
| Alkaline residue (dry net weight) | Concentrated hydrochloric acid (concentration 37%) | Solid product | Carbonic acid gas | Secondary residue |
| 100g | 100g | 105g | 21g | 46g |
Embodiment 2
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 75g, urea 15g, the Sodium Nitrite 10g that prepare by embodiment 1 method.Said components is mixed and can obtain.
Embodiment 3
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 85g, urea 10g, the Sodium Nitrite 5g that prepare by embodiment 1 method.Said components is mixed and can obtain.
Embodiment 4
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 95g, the urea 5g that prepare by embodiment 1 method.Said components is mixed and can obtain.
Embodiment 5
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprising by alkaline residue and acetic acid is the solid product that raw material carries out reacting.
The present embodiment provides the preparation method of this solid product simultaneously, under being included in the condition of stirring, slowly being joined in the retort that alkaline residue has been housed by Glacial acetic acid and reacts, and after reaction carries out 5-6 hour, detects pH; To regulate in retort pH when 7-8 with alkaline residue, Glacial acetic acid, stopped reaction, must be suspended the reaction solution of state, then carries out vacuum filtration, vacuum tightness 15kPa, evaporation, dry, obtained solid product.This solid product directly can be used as environment protection snow-dissolved agent.The byproduct carbonic acid gas of reaction is reclaimed in reaction process.
Its reaction formula is:
CaCO
3+2CH
3COOH＝(CH
3COO)
2Ca+H
2O+CO
2↑
Ca(OH)
2+2CH
3COOH＝(CH
3COO)
2Ca+2H
2O
The present embodiment Raw charging capacity and product amount see the following form 2
Table 2
| Alkaline residue (dry net weight) | Glacial acetic acid | Solid product | Carbonic acid gas | Secondary residue |
| 100g | 60g | 100g | 20g | 40g |
Embodiment 6
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 10g, the magnesium acetate 90g that prepare by embodiment 5 method.Said components is mixed and can obtain.
Embodiment 7
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 20g, the magnesium acetate 80g that prepare by embodiment 5 method.Said components is mixed and can obtain.
Embodiment 8
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 30g, the magnesium acetate 70g that prepare by embodiment 5 method.Said components is mixed and can obtain.
Embodiment 9
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 40g, the magnesium acetate 60g that prepare by embodiment 5 method.Said components is mixed and can obtain.
Embodiment 10
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises the solid product 50g, the magnesium acetate 50g that prepare by embodiment 5 method.Said components is mixed and can obtain.
Embodiment 11-15
Several environment protection snow-dissolved agent utilizing alkaline residue to prepare is provided, comprises solution (20%wt) and the magnesium acetate solution (20%wt) of the solid product prepared by embodiment 5 method; The two volume ratio is as shown in table 3 below.Said components is mixed and can obtain.
Table 3
Embodiment 16
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprising by alkaline residue and hydrochloric acid and Glacial acetic acid is the solid product that raw material carries out reacting.
The present embodiment provides the preparation method of this solid product simultaneously, under being included in the condition of stirring, hydrochloric acid and Glacial acetic acid slowly being joined in the retort that alkaline residue has been housed and reacts, and after reaction carries out 5-6 hour, detects pH; To regulate in retort pH when 7-8 with alkaline residue, concentrated hydrochloric acid or Glacial acetic acid, stopped reaction, must be suspended the reaction solution of state, then carries out vacuum filtration, vacuum tightness 15kPa, evaporation, dry, obtained solid product.This solid product directly can be used as environment protection snow-dissolved agent.The byproduct carbonic acid gas of reaction is reclaimed in reaction process.
Its reaction formula is:
CaCO
3+2HCl＝CaCl
2+H
2O+CO
2↑
Ca(OH)
2+2HCl＝CaCl
2+2H
2O
CaCO
3+2CH
3COOH＝(CH
3COO)
2Ca+H
2O+CO
2↑
Ca(OH)
2+2CH
3COOH＝(CH
3COO)
2Ca+2H
2O
The present embodiment Raw charging capacity and product amount see the following form 4.
Table 4
Embodiment 17
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises solid product 77.5 parts, 9 parts, urea, Sodium Nitrite 4.5 parts, the magnesium acetate 9 parts prepared by numbering 1 method in embodiment 16.Said components is mixed and can obtain.
Embodiment 18
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises solid product 70 parts, 8 parts, urea, Sodium Nitrite 4 parts, the magnesium acetate 18 parts prepared by numbering 2 in embodiment 16.Said components is mixed and can obtain.
Embodiment 19
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises solid product 62.5 parts, 7 parts, urea, Sodium Nitrite 3.5 parts, the magnesium acetate 27 parts prepared by numbering 3 in embodiment 16.Said components is mixed and can obtain.
Embodiment 20
The present embodiment provides a kind of environment protection snow-dissolved agent utilizing alkaline residue to prepare, and comprises solid product 55 parts, 6 parts, urea, Sodium Nitrite 3 parts, the magnesium acetate 36 parts prepared by numbering 4 in embodiment 16.Said components is mixed and can obtain.
Experimental example 1
According to the detection to the environment protection snow-dissolved agent snow removing ice-melt effect that embodiment 1-4 obtains of the national standard of GBT23851-2009 " road deicing Snow Agent ", the results are shown in following table 5.
Concrete detecting step is as follows: under the same terms, and the sodium chloride solution of preparation same concentrations, as reference solution; Get the porcelain crucible of the identical diameter of two 150mL and height, add 100mL water, label 1 and 2, put in the cryostat of-10 ± 1 DEG C, freeze; Pipette 25mL Snow Agent (Snow Agent) solution and sodium chloride solution respectively in 50mL beaker, in-10 ± 1 DEG C of thermostat container, for subsequent use after 12 hours; Take out the porcelain crucible of ice cube, dry outer wall, weigh rapidly, note m
01and m
02; Poured into by the Snow Agent solution prepared in No. 1 porcelain crucible, sodium chloride solution is poured in No. 2 porcelain crucibles, after be put in 0.5h in cryostat.Take out, pouring liquid, weighs residual mass rapidly, note m
1and m
2.
Deicing or snow melting ability represents with W:
Table 5
| Laboratory sample | Snow removing ice-melt effect |
| Embodiment 1 | 65％ |
| Embodiment 2 | 70％ |
| Embodiment 3 | 95％ |
| Embodiment 4 | 90％ |
| Sodium-chlor | 100％ |
| Calcium chloride (nodeless mesh water) | 135％ |
Find through abundant experimental results, environment protection snow-dissolved agent prepared by embodiment 3 has good snow melt deicing effect, reaches 95% of same concentration sodium-chlor.
Experimental example 2
Carry out XRD (i.e. X-ray diffraction) composition analysis to the environment protection snow-dissolved agent (i.e. solid product) obtained by embodiment 1, result as shown in Figure 1.Analyze known, product is CaCl
24H
2the mixture of O and NaCl.By XRD semi-quantitative analysis, CaCl
24H
2the output of O reaches more than 95%.
Experimental example 3
According to the detection to the environment protection snow-dissolved agent snow removing ice-melt effect that embodiment 5-10 obtains of the national standard of GBT23851-2009 " road deicing Snow Agent ", the results are shown in following table 6.Concrete detection method is with experimental example 1.
Table 6
| Laboratory sample | Snow removing ice-melt effect |
| Embodiment 5 | 54％ |
| Embodiment 6 | 75％ |
| Embodiment 7 | 68％ |
| Embodiment 8 | 65％ |
| Embodiment 9 | 62％ |
| Embodiment 10 | 60％ |
| Sodium-chlor | 100％ |
| Calcium acetate | 55％ |
Find through abundant experimental results, environment protection snow-dissolved agent prepared by embodiment 5-10, snow melt deicing effect is at more than 60% of same concentration sodium-chlor.The advantage of environment protection snow-dissolved agent prepared by embodiment 5-10 is environmental protection, compared with traditional Snow Agent sodium-chlor, greatly reduces the corrosion condition to metal and road surface, and significantly reduces the production cost of Snow Agent.
Experimental example 4
Carry out XRD (i.e. X-ray diffraction) composition analysis to the environment protection snow-dissolved agent (i.e. solid product) obtained by embodiment 5, result as shown in Figure 2.Analyze known, product is (CH
3cOO)
2caH
2the mixture of O and NaCl.By XRD semi-quantitative analysis, (CH
3cOO)
2caH
2the output of O reaches more than 65%.
Experimental example 5 corrodibility contrast experiment
Think in theory, sodium-chlor and calcium chloride have corrosive nature to metal, but degree is different, and under same concentrations, the corrodibility of calcium chloride is 50% of sodium-chlor.In order to show corrosive effect more intuitively further, this experiment compares the corrosion condition of drawing pin of sodium-chlor process 48h of environment protection snow-dissolved agent obtained through the embodiment 1 of distilled water, 20% (wt) respectively, 20% (wt).The results are shown in Figure 3.Experiment finds, the drawing pin surface corrosion through sodium-chlor process is serious, and comparatively light through the drawing pin corrosion of the obtained environment protection snow-dissolved agent process of embodiment 1, similar with the situation of distilled water process.
Experimental example 6
According to the detection to the environment protection snow-dissolved agent snow removing ice-melt effect that numbering 1-4 and embodiment 17-20 in embodiment 16 obtains of the national standard of GBT23851-2009 " road deicing Snow Agent ", the results are shown in following table 7.Concrete detection method is with experimental example 1.
Table 7
| Laboratory sample | Snow removing ice-melt effect |
| Embodiment 16 numbering 1 | 72％ |
| Embodiment 16 numbering 2 | 70％ |
| Embodiment 16 numbering 3 | 69％ |
| Embodiment 16 numbering 4 | 66％ |
| Embodiment 17 | 97％ |
| Embodiment 18 | 95％ |
| Embodiment 19 | 90％ |
| Embodiment 20 | 83％ |
| Sodium-chlor | 100％ |
| Calcium acetate | 55％ |
| Calcium chloride (nodeless mesh water) | 135％ |
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. the environment protection snow-dissolved agent utilizing alkaline residue to prepare, comprising by alkaline residue and acid is the product that raw material carries out reacting.
2. environment protection snow-dissolved agent according to claim 1, is characterized in that, described acid is one or more in hydrochloric acid, acetic acid, waste hydrochloric acid, wood vinegar, sulfuric acid; Preferably, described acid is hydrochloric acid and acetic acid.
3. environment protection snow-dissolved agent according to claim 1 and 2, is characterized in that, the content of described alkaline residue neutral and alkali calcium salt is not less than 70%, and preferred described alkaline calcium salt comprises one or more in calcium carbonate, calcium sulfate, calcium chloride.
4. the environment protection snow-dissolved agent according to any one of claim 1-3, it is characterized in that, the preparation method of described product comprises: under the condition stirred, hydrochloric acid and/or acetic acid are joined in the retort that alkaline residue is housed and reacts, then reaction system pH to 7-8 is regulated with described alkaline residue or described acid, the reaction solution of state must be suspended, filter, obtain liquid product;
Or further by described liquid product through evaporation, dry, obtain solid product.
5. environment protection snow-dissolved agent according to claim 4, is characterized in that, the time of carrying out in retort described in the preparation method of described product reacting is 5-6 hour.
6. environment protection snow-dissolved agent according to claim 4, is characterized in that, is filtered into vacuum filtration described in the preparation method of described product, and preferred vacuum tightness is 1-20kPa.
7. environment protection snow-dissolved agent according to claim 4, is characterized in that, also comprises the clear liquid after to filtration and carry out desolventing technology in the preparation method of described product; Preferred decoloration treatment method is charcoal absorption decolouring.
8. environment protection snow-dissolved agent according to any one of claim 4-7, is characterized in that, with parts by weight, comprise by alkaline residue and hydrochloric acid be raw material carry out reacting described solid product 75-95 part, urea 5-15 part, Sodium Nitrite 0-10 part.
9. the environment protection snow-dissolved agent according to any one of claim 4-7, is characterized in that, with parts by weight, comprise by alkaline residue and acetic acid be raw material carry out reacting solid product 10-50 part, magnesium acetate 50-90 part.
10. the environment protection snow-dissolved agent according to any one of claim 4-7, it is characterized in that, with parts by weight, comprise by alkaline residue and hydrochloric acid and acetic acid be raw material carry out reacting solid product 50-80 part, urea 6-9 part, Sodium Nitrite 3-4.5 part, magnesium acetate 9-36 part.
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| CN113943549A (en) * | 2021-11-18 | 2022-01-18 | 西安热工研究院有限公司 | Wind power blade ice melting and ice inhibiting agent based on exothermic reaction and preparation method thereof |
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