CN108439843A - A kind of method and its application synthesizing early strength agent with industrial waste nitric acid - Google Patents

A kind of method and its application synthesizing early strength agent with industrial waste nitric acid Download PDF

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Publication number
CN108439843A
CN108439843A CN201810481882.6A CN201810481882A CN108439843A CN 108439843 A CN108439843 A CN 108439843A CN 201810481882 A CN201810481882 A CN 201810481882A CN 108439843 A CN108439843 A CN 108439843A
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China
Prior art keywords
nitric acid
early strength
added
agent
parts
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CN201810481882.6A
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Chinese (zh)
Inventor
宋宝
马丽涛
王浩雨
邢凯
乔琼琼
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Anhui Xin Solid Environmental Co Ltd
Ward Xiao County Chemical Industry Science Co Ltd
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Anhui Xin Solid Environmental Co Ltd
Ward Xiao County Chemical Industry Science Co Ltd
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Priority to CN201810481882.6A priority Critical patent/CN108439843A/en
Publication of CN108439843A publication Critical patent/CN108439843A/en
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B40/00Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
    • C04B40/0028Aspects relating to the mixing step of the mortar preparation
    • C04B40/0039Premixtures of ingredients
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2103/00Function or property of ingredients for mortars, concrete or artificial stone
    • C04B2103/10Accelerators; Activators
    • C04B2103/12Set accelerators

Abstract

The present invention provides a kind of preparation method and applications of industrial waste nitric acid synthesis early strength agent, is related to chemical field, wherein the preparation method of industrial waste nitric acid synthesis early strength agent, includes the following steps:Nitric acid waste is put into four-hole boiling flask, start to stir, slowly put into quick lime, until solution pH value is 78, stop that quick lime is added, reaction can stop, then through filtering, evaporation, crystallization can be obtained four water-calcium nitrate, polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, then foam control agent is added, water is added after stirring, parts by weight are the number surplus of added raw material, after stirring, plasticity-maintaining agent is added, calcium nitrate obtained, after stirring, add triethanolamine, air entraining agent, stirring can be obtained finished product, its application in Prefabricated Concrete is the product that will obtain according to 2.0% 3.0% incorporations of gel material content in concrete mix, the present invention realizes the recycling of industrial waste nitric acid, and realize the application in Prefabricated Concrete.

Description

A kind of method and its application synthesizing early strength agent with industrial waste nitric acid
Technical field
The present invention relates to chemical fields, and in particular to a kind of method and its application synthesizing early strength agent with industrial waste nitric acid.
Background technology
Industrial waste nitric acid, such as the acid pickle of C261-057-34 generations belong to hazardous waste with stronger corrosivity, Be unable to direct emission, recycling waste nitric acid using when also first to go out beavy metal impurity, energy consumption is big, of high cost, so at present seldom There is enterprise to recycle waste nitric acid, one of concrete admixture, concrete early strength agent refers to that can improve early strength of concrete, and right The additive that later strength does not make significant difference, the main function of early strength agent are to accelerate hydrated cementitious speed, promotion concrete early The development of phase intensity;Not only there is early powerful, but also had the function of certain water reducing and strength increasing.Concrete early strength agent is that additive development is gone through One of additive kind used earliest in history.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of in the method for industrial waste nitric acid synthesis early strength agent and its answers With, the recycling of the industrial waste nitric acid of realization, and realize the application in Prefabricated Concrete.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) nitric acid waste is put into four-hole boiling flask, starts to stir, slowly put into quick lime, until solution pH value to 7- 8, stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:150-230 parts of polycarboxylate superplasticizer mother liquor, foam control agent 0.5-1.5 Part, 5-10 parts of plasticity-maintaining agent, 300-500 parts of four water-calcium nitrate, 20-35 parts of triethanolamine, 0.3-1 parts of air entraining agent;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, control is then added Infusion, it is primary to stir, water is then added, plasticity-maintaining agent, calcium nitrate obtained is added in secondary agitation, and triple mixing adds three second Hydramine, air entraining agent, four stirrings can be obtained finished product.
Preferably, the chuck of the additional cooling water of four-hole boiling flask adjusts cooling according to reaction progress situation in step (1) Water consumption reduces the severe degree of reaction.
Preferably, a mixing time described in step (2) is 5-10 minutes, and the secondary agitation time is 5 minutes, institute It is 10-20 minutes to state the triple mixing time, and four mixings time are 10-15 minutes.
Preferably, polycarboxylic acids mother liquor described in step (2) is to synthesize to obtain with isoamyl alcohol polyoxyethylene ether polymeric monomer.
Preferably, plasticity-maintaining agent described in step (2) is minimum one kind in sodium gluconate, citric acid, sodium tripolyphosphate.
Preferably, air entraining agent described in step (2) is triterpenoid saponin.
Preferably, foam control agent described in step (2) is higher alcohols polyethers esters.
Preferably, the solid content of polycarboxylate superplasticizer mother liquor described in step (3) is 40%.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application The 2.0%-3.0% of gel material dosage is mixed.
(3) advantageous effect
The present invention provides a kind of method and its application synthesizing early strength agent with industrial waste nitric acid, have below beneficial to effect Fruit:
First, by the recycling to industrial waste nitric acid, prevent it from polluting and damaging caused by Environmental insults, simultaneously Without carrying out any processing such as other physical chemistry to waste nitric acid, can direct circulation utilize, reduce energy consumption, secondly, utilize industry Waste nitric acid is reacted with quick lime, and product calcium nitrate is good early strength antifreezing agent in concrete, the components such as compounding water-reducing agent The demoulding time of prefabricated components and winter construction concrete can be reduced, mold week transfer efficient is improved, speeds up the work, most Afterwards, its product is applied in concrete by the present invention while efficiently using industrial waste nitric acid, and improves coagulation obtained The quality level of soil is beneficial to energy conservation and environmental protection, realizes sustainable development.
Specific implementation mode
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention, Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making The every other embodiment obtained under the premise of creative work, shall fall within the protection scope of the present invention.
Embodiment 1:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 8, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:180 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 6 parts of sodium gluconate, 300 parts of four water-calcium nitrate, 25 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 8 minutes, sodium gluconate, four water-calcium nitrate is added in secondary agitation 5 minutes, Triple mixing 12 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 13 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.5% incorporation of gel material dosage.
Embodiment 2:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 7, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:200 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 5 parts of citric acid, 400 parts of four water-calcium nitrate, 28 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 8 minutes, citric acid, four water-calcium nitrate is added, three times in secondary agitation 5 minutes Stirring 15 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 13 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.5% incorporation of gel material dosage.
Embodiment 3:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 7, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:190 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 5 parts of citric acid, 350 parts of four water-calcium nitrate, 26 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 7 minutes, citric acid, four water-calcium nitrate is added, three times in secondary agitation 5 minutes Stirring 12 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 15 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.0% incorporation of gel material dosage.
Embodiment 4:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 8, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:185 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 6 parts of sodium gluconate, 320 parts of four water-calcium nitrate, 28 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 6 minutes, sodium gluconate, four water-calcium nitrate is added in secondary agitation 5 minutes, Triple mixing 12 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 10 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.0% incorporation of gel material dosage.
Embodiment 5:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 7, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:195 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 5 parts of citric acid, 360 parts of four water-calcium nitrate, 26 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 9 minutes, citric acid, four water-calcium nitrate is added, three times in secondary agitation 5 minutes Stirring 17 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 11 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.4% incorporation of gel material dosage.
Embodiment 6:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 8, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:190 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 6 parts of sodium gluconate, 330 parts of four water-calcium nitrate, 32 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 6 minutes, sodium gluconate, four water-calcium nitrate is added in secondary agitation 5 minutes, Triple mixing 12 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 13 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.2% incorporation of gel material dosage.
Embodiment 7:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 7, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:186 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 5 parts of citric acid, 330 parts of four water-calcium nitrate, 25.5 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 6 minutes, citric acid, four water-calcium nitrate is added, three times in secondary agitation 5 minutes Stirring 10 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 15 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.7% incorporation of gel material dosage.
Embodiment 8:
A method of early strength agent is synthesized with industrial waste nitric acid, is included the following steps:
(1) by nitric acid waste put into four-hole boiling flask in, start to stir, slowly put into quick lime, until solution pH value be 8, Stop that quick lime is added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:188 parts of polycarboxylate superplasticizer mother liquor, 0.8 part of higher alcohols polyether ester, 6 parts of sodium gluconate, 360 parts of four water-calcium nitrate, 29 parts of triethanolamine, 0.5 part of triterpenoid saponin;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, is then added high Then water is added in carbon alcohol polyether ester, primary stirring 7 minutes, sodium gluconate, four water-calcium nitrate is added in secondary agitation 5 minutes, Triple mixing 17 minutes, adds triethanolamine, triterpenoid saponin, and four stirrings can be obtained finished product in 13 minutes.
Above-mentioned early strength agent can be applied in Prefabricated Concrete, by the early strength agent according to glue in concrete mix when application 2.1% incorporation of gel material dosage.
Table 2 is concrete prepared by 1-2 of the embodiment of the present invention, respectively with blank item coagulation that water-reducing agent is not added Soil, the comparative run concrete that ordinary water-reducing agent is added, in the performance test of demoulding time, intensity etc., and by test result It is recorded in table 2, wherein water-reducing agent is mixed according to concrete mix shown in table 1.
1 concrete mix of table
2 performance comparison of table
As seen from the above table, the concrete that prepared by 1-2 of the embodiment of the present invention effectively shortens demoulding time, and 1d, 7d, Concrete strength when 28d is above blank item and ordinary water-reducing agent comparative run, and the present invention utilizes waste nitric acid and quick lime Reaction generates calcium nitrate, and compounding is in concrete, improving all transfer efficients of mold, accelerating project progress, solve simultaneously Harm of the nitric acid waste to Environmental insults.
It should be noted that herein, relational terms such as first and second and the like are used merely to a reality Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those Element, but also include other elements that are not explicitly listed, or further include for this process, method, article or equipment Intrinsic element.In the absence of more restrictions, the element limited including sentence "including a ...", it is not excluded that There is also other identical elements in the process, method, article or apparatus that includes the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations, although with reference to the foregoing embodiments Invention is explained in detail, it will be understood by those of ordinary skill in the art that:It still can be to aforementioned each implementation Technical solution recorded in example is modified or equivalent replacement of some of the technical features;And these modification or It replaces, the spirit and scope for various embodiments of the present invention technical solution that it does not separate the essence of the corresponding technical solution.

Claims (9)

1. a kind of method synthesizing early strength agent with industrial waste nitric acid, which is characterized in that include the following steps:
(1) nitric acid waste is put into four-hole boiling flask, starts to stir, slowly put into quick lime, until solution pH value to 7-8, stops Quick lime is only added, reaction can stop, and then can be obtained four water-calcium nitrate through filtering, evaporation, crystallization;
(2) following component is weighed according to parts by weight:150-230 parts of polycarboxylate superplasticizer mother liquor, is protected 0.5-1.5 parts of foam control agent Mould 5-10 parts of agent, 300-500 parts of four water-calcium nitrate, 20-35 parts of triethanolamine, 0.3-1 parts of air entraining agent;
(3) polycarboxylate superplasticizer mother liquor is added in the four-hole boiling flask equipped with stirring according to parts by weight, foam control agent is then added, Primary stirring, is then added water, secondary agitation, is added plasticity-maintaining agent, calcium nitrate obtained, triple mixing, add triethanolamine, Air entraining agent, four stirrings can be obtained finished product.
2. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that step (1) Zhong Sikou The chuck of the additional cooling water of flask carries out situation according to reaction, adjusts cooling water amount, reduce the severe degree of reaction.
3. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (2) Mixing time is 5-10 minutes, and the secondary agitation time is 5 minutes, and the triple mixing time is 10-20 minutes, institute It is 10-15 minutes to state four mixings time.
4. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (2) Polycarboxylic acids mother liquor is to synthesize to obtain with isoamyl alcohol polyoxyethylene ether polymeric monomer.
5. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (2) Plasticity-maintaining agent is minimum one kind in sodium gluconate, citric acid, sodium tripolyphosphate.
6. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (2) Air entraining agent is triterpenoid saponin.
7. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (2) Foam control agent is higher alcohols polyethers esters.
8. the method for synthesizing early strength agent as described in claim 1 with industrial waste nitric acid, which is characterized in that described in step (3) The solid content of polycarboxylate superplasticizer mother liquor is 40%.
9. the application of early strength agent is synthesized with industrial waste nitric acid as described in claim 1, which is characterized in that the early strength agent can be with It is applied in Prefabricated Concrete, by the early strength agent according to the 2.0%- of gel material content in concrete mix when application 3.0% incorporation.
CN201810481882.6A 2018-05-18 2018-05-18 A kind of method and its application synthesizing early strength agent with industrial waste nitric acid Pending CN108439843A (en)

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Application publication date: 20180824