CN103833249A - Chromium removal enhancer and preparation method thereof - Google Patents
Chromium removal enhancer and preparation method thereof Download PDFInfo
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Abstract
The invention provides a method for preparing a chromium removal enhancer. The method comprises the following steps: (a) calcining kaolin, mixing the calcined kaolin and an acid solution, performing suction filtration, and washing and drying the obtained solid; (b) mixing the kaolin obtained in the step (a) and an mixed solution, and reacting to obtain the chromium removal enhancer, wherein the mixed solution is a mixed solution of a reducing agent, an antioxidant, an enhancer and water. According to the chromium removal enhancer prepared by the invention, the kaolin is taken as a raw material, the reducing agent, the antioxidant and the enhancer are mixed with the modified kaolin, and the chromium removal enhancer is obtained after the reaction. According to the chromium removal enhancer prepared by the invention, due to dual effects of adsorption and reduction, hexavalent chromium in cement is effectively removed, and physical properties of the cement are improved. The invention also provides the chromium removal enhancer prepared according to the method.
Description
Technical field
The present invention relates to objectionable impurities in cement and remove technical field, relate in particular to a kind of dechromisation toughener and preparation method thereof.
Background technology
Chromium is a kind of argenteous hard metal, mainly occurs with chromium metal, trivalent chromium and three kinds of forms of sexavalent chrome.The compound of chromium is nearly all toxic, wherein sexavalent chrome toxicity maximum.Sexavalent chrome is the property swallowed or imbedibility poisonous substance, is mainly chronic murder by poisoning to human body, and it can pass through digestive tube, respiratory tract, skin and mucous membrane and invade human body; And sexavalent chrome has strong oxidation, therefore chromic chronic poisoning often starts to develop into gradually incurable with local lesion.
In the raw material of cement and production process, all can produce sexavalent chrome, the sexavalent chrome in cement equally also can produce serious detrimentally affect to human body, and skin pain is festered, and forms the cement dermatitis or the cement eczema that are difficult to healing.In June, 2003, European Union promulgates instruction, forbids on market selling and using water-soluble content of 6-valence Cr ions to exceed 0.0002% cement and cement products; 2006 7
Month, European standard ENl96.10-2006 issuing and implementation.In recent years, the hexavalent chromium polluted problem of cement has also caused the great attention of relevant department.But in cement and concrete, dechromisation special assistant is also rarely found.
Publication number is that the Chinese patent of CN101282917A discloses a kind of liquid chromium remover for cement, it comprises can hydrated cementitious particle and be incorporated into the metal matrix chromium reducing agent in cement granules with the form of association complex, and association complex is the form formation with non-sulfonated lignin base complex by metal matrix chromium reducing agent.This liquid chromium remover dechromisation effect is not very remarkable, is secondly its easily oxidized reductive action that loses of reductive agent in preservation and use procedure.
Kaolin is a kind of natural non-metallic minerals, has abundant reserves in China, is widely used in the field such as chemical industry, building materials.Kaolin has the physico-chemical property such as cation exchange capacity (CEC), good resistivity against fire, of many uses.Thus, the application provides a kind of dechromisation toughener taking kaolin as raw material.
Summary of the invention
The technical problem that the present invention solves is to provide good dechromisation toughener of a kind of dechromisation effect and preparation method thereof.
In view of this, the application provides a kind of preparation method of dechromisation toughener, comprises the following steps:
A) kaolin is calcined, the kaolin after calcining is mixed with acidic solution, then carry out suction filtration, by dry after the solids wash obtaining;
B) kaolin step a) being obtained mixes with mixed solution, obtains dechromisation toughener after reaction; Described mixed solution is the mixed solution of reductive agent, antioxidant, toughener and water.
Preferably, the temperature of described calcining is 800～900 DEG C, and the time of described calcining is 2h～4h.
Preferably, described acidic solution is hydrochloric acid, sulfuric acid or phosphoric acid.
Preferably, described reductive agent is ferrous sulfate, iron protochloride, stannous sulfate or tin protochloride.
Preferably, described antioxidant is citric acid, xitix or oxalic acid.
Preferably, described toughener is sodium-chlor, calcium chloride, sodium sulfate, trolamine or tri-isopropanolamine.
Preferably, the concentration of described acidic solution is 0.1mol/L～0.5mol/L.
The dechromisation toughener that the application also provides the preparation method described in such scheme to prepare.
Preferably, described dechromisation toughener comprises:
Reductive agent 10wt%～20wt%;
Antioxidant 1wt%～5wt%;
Toughener 20wt%～30wt%;
Kaolin surplus.
Preferably, the content of described reductive agent is 12wt%～17wt%, and the content of described antioxidant is 2wt%～3wt%, and the content of described toughener is 22wt%～27wt%.
The application provides a kind of preparation method of dechromisation toughener.Preparing in the process of dechromisation toughener, first kaolin is calcined, then the kaolin after calcining is mixed with acidic solution, in acidic solution, carry out modification, finally kaolin after treatment is mixed with reductive agent, antioxidant, toughener, after reaction, obtain dechromisation toughener.
Kaolinic basic structure is silicon-oxy tetrahedron and alumina octahedral, after kaolin calcined, can increase its surface-area, pore volume, and silicon-dioxide and alchlor content all increase, active site increases, kaolinic said structure after calcining makes it have good gelation activity, be conducive to the hydration of cement and increase the each age strength of cement, and thering is the performance of adsorbing various ions and impurity from surrounding medium; Kaolin after calcining, through acid solution processing, can be widened kaolinic mesopore aperture, and form new surface microporous structure, and pore size distribution is disperse more, and mean pore size increases, and pore volume and specific surface area increase, and the adsorptive power of chromium ion is improved greatly; Reductive agent is reduction of hexavalent chromium effectively; Reductive agent loads on kaolin and can fully contact with cement simultaneously, to greatest extent chromium is reduced; Antioxidant reduces the oxidation of reductive agent in preparation and preservation process, ensures the reduction effect of reductive agent; Toughener can effectively improve the physicals of cement, promotes the hydration process of cement, and the each age strength of cement is all improved.In sum, dechromisation toughener prepared by the present invention, by the dual function of adsorbing and reducing, is effectively removed the sexavalent chrome in cement, improves the physicals of cement simultaneously.
Embodiment
In order further to understand the present invention, below in conjunction with embodiment, the preferred embodiment of the invention is described, but should be appreciated that these are described is for further illustrating the features and advantages of the present invention, instead of limiting to the claimed invention.
The preparation method who the embodiment of the invention discloses a kind of dechromisation toughener, comprises the following steps:
A) kaolin is calcined, the kaolin after calcining is mixed with acidic solution, then carry out suction filtration, by dry after the solids wash obtaining;
B) kaolin step a) being obtained mixes with mixed solution, obtains dechromisation toughener; Described mixed solution is the mixed solution of reductive agent, antioxidant, toughener and water.
The application provides a kind of dechromisation toughener and preparation method thereof, and described dechromisation toughener is taking modified kaolin as carrier, for removing the chromic toughener of cement or concrete.Toughener provided by the invention, under the dual function of absorption and reduction, can effectively be removed the sexavalent chrome harm to human body and environment with minimizing in cement, and this toughener can also effectively improve the physicals of cement simultaneously.
Preparing in the process of dechromisation toughener, first the application has carried out modification by kaolin.Kaolin of the present invention is a kind of natural non-metallic minerals, and its basic structure is silicon-oxy tetrahedron and aluminum-oxygen tetrahedron.First the application calcines kaolin, and in kaolin calcined process, the various impurity in kaolin aperture are removed, thereby have widened kaolinic aperture, have increased kaolinic microvoid structure; On the other hand, calcining makes kaolinic structure that change occur, and Al is the activated four-coordination of tool and pentacoordinate by the hexa-coordinate structural transformation of inertia, has produced a large amount of active silicas simultaneously.
The kaolinic structure obtaining through calcining makes it have good gelation activity, is conducive to the hydration of cement and increases the cement intensity in each length of time; Kaolin also has the performance of adsorbing various ions and impurity from surrounding medium simultaneously, and in solution, has ion-exchange character.The temperature of calcining described in the application is preferably 800 DEG C～900 DEG C, more preferably 850 DEG C～880 DEG C; The time of described calcining is preferably 2h～4h, more preferably 3h～3.5h.
According to the present invention, kaolin is after high-temperature calcination, the kaolin after calcining is carried out acid treatment by the application, the kaolin being about to after calcining mixes with acidic solution, kaolin after calcining is carried out to modification in acidic solution, then carry out suction filtration, make solid-liquid separation, by dry after the solids wash after solid-liquid separation, obtain the kaolin after modification.Described acidic solution is preferably hydrochloric acid, sulfuric acid or phosphoric acid.The concentration of described acidic solution is preferably 0.1mol/L～0.5mol/L, more preferably 0.1mol/L～0.3mol/L.The detailed process that kaolin after calcining is processed in acidic solution is:
Kaolin after calcining is added in acidic solution, stirs 4h～5h at 80 DEG C～100 DEG C, then carry out suction filtration, will be dry after the solids wash obtaining.
Kaolin after calcining can be widened kaolinic mesopore aperture through the processing of acidic solution, increase volume large, mesopore, and form some new surface microporous structures, pore size distribution is disperse more, mean pore size increases, pore volume and specific surface area increase, and the adsorptive power of chromium ion is improved greatly.In summary, kaolin makes kaolinic structure that above-mentioned change occur through modification, thereby has greatly improved the adsorptive power of the kaolin after modification to chromium.
Then the present invention mixes the kaolin after modification with reductive agent, antioxidant, toughener, water, obtain dechromisation toughener after reaction.Described in the application, reductive agent is preferably ferrous sulfate, iron protochloride, stannous sulfate or tin protochloride; Described antioxidant is preferably water soluble antioxidant, more preferably citric acid, xitix or oxalic acid; Described toughener is preferably inorganic salt or organic toughener, and described inorganic salt are preferably sodium-chlor, calcium chloride or sodium sulfate, and described organic toughener is preferably trolamine or tri-isopropanolamine.After kaolin, reductive agent, antioxidant, toughener mix with water described in the application, there is ion-exchange and complex reaction, thereby obtained dechromisation toughener.
Above-mentioned reductive agent is reduction of hexavalent chromium effectively, makes chromic content meet standard-required, and reductive agent can load on kaolin and fully contact with cement, to greatest extent chromium is reduced.Antioxidant can reduce the oxidation of reductive agent in preparation and preservation process, further ensures the reduction effect of reductive agent.And toughener can improve the physical properties of cement, promote the hydration process of cement, cement is all improved at each age strength.Therefore, the application mixes the kaolin after modification with reductive agent, antioxidant, toughener after, the dechromisation toughener obtaining can be reduced chromium to greatest extent, and can reduce the oxidation of reductive agent in preparation and preservation process, make dechromisation toughener there is higher stability, and can improve the physical properties of cement.
According to the present invention, for the kaolin after modification can be mixed with antioxidant, reductive agent, toughener, as preferred method, the preparation process of described dechromisation toughener is specially:
Reductive agent, antioxidant, toughener and water are mixed with to mixed solution;
Kaolin through modification is mixed with described mixed solution, stir 2h～3h, suction filtration, air-dry rear pulverizing, obtains dechromisation toughener.
The application provides a kind of preparation method of dechromisation toughener.Preparing in the process of dechromisation toughener, first kaolin is calcined, then the kaolin after calcining is processed in acidic solution, finally kaolin after treatment is mixed with reductive agent, antioxidant, toughener, obtain dechromisation toughener.Kaolinic basic structure is silicon-oxy tetrahedron and alumina octahedral, can increase its surface-area, pore volume after kaolin calcined, has stronger ion adsorption; Kaolin after calcining, through acid solution processing, has further improved the adsorptive power to chromium ion; And effectively reduction of hexavalent chromium of reductive agent; Reductive agent loads on kaolin and can fully contact with cement simultaneously, to greatest extent chromium is reduced; Antioxidant reduces the oxidation of reductive agent in preparation and preservation process, ensures the stability of reductive agent; Toughener can effectively improve the physicals of cement, promotes the hydration process of cement, and the each age strength of cement is all improved.In sum, dechromisation toughener of the present invention, by the dual function of adsorbing and reducing, is effectively removed the sexavalent chrome in cement, and makes dechromisation toughener have higher stability.
The application also provides the dechromisation toughener prepared by aforesaid method, and as preferred version, described dechromisation toughener comprises:
Reductive agent 10wt%～20wt%;
Antioxidant 1wt%～5wt%;
Toughener 20wt%～30wt%;
Kaolin surplus.
According to the present invention, described in dechromisation toughener, reductive agent is preferably ferrous sulfate, iron protochloride, stannous sulfate or tin protochloride; Described antioxidant is preferably water soluble antioxidant, more preferably citric acid, xitix or oxalic acid; Described toughener is preferably inorganic salt or organic toughener, and described inorganic salt are preferably sodium-chlor, calcium chloride or sodium sulfate, and described organic toughener is preferably trolamine or tri-isopropanolamine.The content of reductive agent, kaolin, antioxidant and toughener in the toughener of dechromisation described in the application, can carry out suitable adjustment according to chromic content in cement or concrete.As preferred version, the content of described reductive agent is preferably 12wt%～17wt%, more preferably 14wt%～16wt%.The content of described antioxidant is preferably 1.8wt%～4wt%, more preferably 2wt%～3wt%.The content of described toughener is 22wt%～27wt%, more preferably 24wt%～26wt%.
In order further to understand the present invention, below in conjunction with embodiment, dechromisation toughener provided by the invention and preparation method thereof is elaborated, protection scope of the present invention is not limited by the following examples.
Raw material in following examples is commercially available prod.
Embodiment 1
(1) kaolin is calcined to 3h at 850 DEG C;
(2) under agitation condition, the kaolin after calcining is joined in the sulphuric acid soln of 0.1mol/L, stir 4h at 80 DEG C, suction filtration, washing, dries stand-by;
(3) sodium-chlor of the citric acid of the ferrous sulfate of 15wt%, 3wt%, 25wt% is joined to the mixed solution that is mixed with 500mL in deionized water;
(4) getting step 2) the kaolinic 57wt% that obtains joins in the mixed solution of step 3) preparation, continuously stirring 2h, suction filtration, natural air drying, pulverizes, and makes dechromisation toughener.
In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.Detect the dechromisation toughener prepared of the present embodiment, do not add the removal efficiency of chrome of dechromisation toughener prepared by dechromisation toughener and comparative example 1, as shown in table 1, table 1 is the data sheet of embodiment and comparative example dechromisation toughener dechromisation effect.
Embodiment 2
(1) kaolin is calcined to 4h at 900 DEG C;
(2) under agitation the kaolin after calcining is joined in the hydrochloric acid soln of 0.15mol/L, stir 4h at 80 DEG C, suction filtration, washing, dries stand-by;
(3) calcium chloride of the xitix of the iron protochloride of 10wt%, 1wt%, 20wt% is joined to the mixed solution that is mixed with 500mL in deionized water;
(4) getting step 2) the kaolinic 69wt% that obtains joins in the mixed solution of step 3) preparation, continuously stirring 2h, suction filtration, natural air drying, pulverizes, and makes dechromisation toughener.
In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.Detect the dechromisation toughener prepared of the present embodiment, do not add the removal efficiency of chrome of dechromisation toughener prepared by dechromisation toughener and comparative example 1, as shown in table 1, table 1 is the data sheet of embodiment and comparative example dechromisation toughener dechromisation effect.
Embodiment 3
(1) kaolin is calcined to 3.5h at 860 DEG C;
(2) under agitation the kaolin after calcining is joined in the hydrochloric acid soln of 0.25mol/L, stir 4h at 80 DEG C, suction filtration, washing, dries stand-by;
(3) sodium sulfate of the oxalic acid of the tin protochloride of 20wt%, 5wt%, 30wt% is joined to the mixed solution that is mixed with 500mL in deionized water;
(4) getting step 2) the kaolinic 45wt% that obtains joins in the mixed solution of step 3) preparation, continuously stirring 2h, suction filtration, natural air drying, pulverizes, and makes dechromisation toughener.
In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.Detect the dechromisation toughener prepared of the present embodiment, do not add the removal efficiency of chrome of dechromisation toughener prepared by dechromisation toughener and comparative example 1, as shown in table 1, table 1 is the data sheet of embodiment and comparative example dechromisation toughener dechromisation effect.
Embodiment 4
(1) kaolin is calcined to 3.8h at 880 DEG C;
(2) under agitation the kaolin after calcining is joined in the phosphoric acid solution of 0.5mol/L, stir 4h at 80 DEG C, suction filtration, washing, dries stand-by;
(3) calcium chloride of the citric acid of the stannous sulfate of 18wt%, 4wt%, 22wt% is joined to the mixed solution that is mixed with 500mL in deionized water;
(4) getting step 2) the kaolinic 56wt% that obtains joins in the mixed solution of step 3) preparation, continuously stirring 2h, suction filtration, natural air drying, pulverizes, and makes dechromisation toughener.
In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.Detect the dechromisation toughener prepared of the present embodiment, do not add the removal efficiency of chrome of dechromisation toughener prepared by dechromisation toughener and comparative example 1, as shown in table 1, table 1 is the data sheet of embodiment and comparative example dechromisation toughener dechromisation effect.
Comparative example 1
(1) sodium-chlor of the citric acid of the ferrous sulfate of massfraction 15%, 3wt%, 25wt% is joined to the mixed solution liquid that is mixed with 500mL in deionized water.
(2) kaolin of getting 57wt% joins in mixed solution, continuously stirring 2h, and suction filtration, natural air drying, pulverizes, and makes dechromisation toughener.
In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.In cement, the mensuration of chromium content adopts diphenyl carbazide spectrophotometry to measure.Detect the dechromisation toughener prepared of the embodiment of the present invention, do not add the removal efficiency of chrome of dechromisation toughener prepared by dechromisation toughener and comparative example 1, as shown in table 1, table 1 is the data sheet of embodiment and comparative example dechromisation toughener dechromisation effect.
The data sheet of the removal efficiency of chrome of table 1 embodiment of the present invention and comparative example dechromisation toughener
| Group | Dechromisation toughener consumption/% | Chromium clearance/% |
| Embodiment 1 | 0.03 | 99.4 |
| Embodiment 2 | 0.03 | 99.5 |
| Embodiment 3 | 0.03 | 99.6 |
| Embodiment 4 | 0.03 | 99.3 |
| Blank example | 0 | 0 |
| Comparative example 1 | 0.03 | 82 |
In cement, add the dechromisation toughener that the embodiment of the present invention 1, comparative example 1 obtain and do not add dechromisation toughener, the performance of test cement, the application tests in the little mill of φ 500mm × 500mm standard test, the material proportion of cement is: the grog of 46.0wt%, the gypsum of 4.0wt% and 50.0% slag, experimental result is as shown in table 2.
The performance data table of the cement that table 2 embodiment of the present invention and comparative example obtain
From experimental result, after adding dechromisation toughener prepared by the present invention, the solubility content of 6-valence Cr ions in cement reduces greatly, and the physical properties of cement meets standard-required simultaneously, and ultimate compression strength and folding strength all increased and improved each length of time.
The explanation of above embodiment is just for helping to understand method of the present invention and core concept thereof.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, can also carry out some improvement and modification to the present invention, these improvement and modification also fall in the protection domain of the claims in the present invention.
To the above-mentioned explanation of the disclosed embodiments, make professional and technical personnel in the field can realize or use the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiment, General Principle as defined herein can, in the situation that not departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention will can not be restricted to these embodiment shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (10)
1. a preparation method for dechromisation toughener, comprises the following steps:
A) kaolin is calcined, the kaolin after calcining is mixed with acidic solution, then carry out suction filtration, by dry after the solids wash obtaining;
B) kaolin step a) being obtained mixes with mixed solution, obtains dechromisation toughener after reaction; Described mixed solution is the mixed solution of reductive agent, antioxidant, toughener and water.
2. preparation method according to claim 1, is characterized in that, the temperature of described calcining is 800～900 DEG C, and the time of described calcining is 2h～4h.
3. preparation method according to claim 1, is characterized in that, described acidic solution is hydrochloric acid, sulfuric acid or phosphoric acid.
4. preparation method according to claim 1, is characterized in that, described reductive agent is ferrous sulfate, iron protochloride, stannous sulfate or tin protochloride.
5. preparation method according to claim 1, is characterized in that, described antioxidant is citric acid, xitix or oxalic acid.
6. preparation method according to claim 1, is characterized in that, described toughener is sodium-chlor, calcium chloride, sodium sulfate, trolamine or tri-isopropanolamine.
7. preparation method according to claim 1, is characterized in that, the concentration of described acidic solution is 0.1mol/L～0.5mol/L.
8. the dechromisation toughener that prepared by the preparation method described in claim 1～7 any one.
9. dechromisation toughener according to claim 8, is characterized in that, described dechromisation toughener comprises:
Reductive agent 10wt%～20wt%;
Antioxidant 1wt%～5wt%;
Toughener 20wt%～30wt%;
The kaolin of surplus.
10. dechromisation toughener according to claim 9, is characterized in that, the content of described reductive agent is 12wt%～17wt%, and the content of described antioxidant is 2wt%～3wt%, and the content of described toughener is 22wt%～27wt%.
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| CN104496243B (en) * | 2014-11-06 | 2017-03-22 | 中国建筑材料科学研究总院 | Hexavalent chromium reducing agent and preparation method thereof, cement and preparation method thereof |
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| CN105198260A (en) * | 2015-10-13 | 2015-12-30 | 云南锡业股份有限公司 | Special tin-containing additive for removing hexavalent chromium from cement and preparation method of additive |
| CN108585597A (en) * | 2018-07-24 | 2018-09-28 | 青神鑫统领建材有限公司 | A kind of reduction of hexavalent chromium type grinding aid and preparation method thereof |
| CN108585597B (en) * | 2018-07-24 | 2020-10-27 | 青神鑫统领建材有限公司 | Reduced hexavalent chromium type grinding aid and preparation method thereof |
| CN110316992B (en) * | 2019-04-04 | 2020-09-01 | 清华大学 | Steel slag-based cement hexavalent chromium solid reducing agent |
| CN110316992A (en) * | 2019-04-04 | 2019-10-11 | 清华大学 | A kind of steel slag base cement Cr VI solid reductant |
| CN112374789A (en) * | 2020-10-13 | 2021-02-19 | 唐山冀东水泥外加剂有限责任公司 | Cement hexavalent chromium reducing agent and preparation method thereof |
| CN112374789B (en) * | 2020-10-13 | 2022-05-24 | 唐山冀东水泥外加剂有限责任公司 | Cement hexavalent chromium reducing agent and preparation method thereof |
| CN112500014A (en) * | 2020-11-20 | 2021-03-16 | 华润水泥技术研发有限公司 | Preparation method of hexavalent chromium reducing agent for high-temperature-resistant cement |
| CN112500013A (en) * | 2020-11-20 | 2021-03-16 | 华润水泥技术研发有限公司 | Preparation method of nano-loaded hexavalent chromium reducing agent for cement |
| CN113548680A (en) * | 2021-08-25 | 2021-10-26 | 北京金隅北水环保科技有限公司 | Method and system for dechlorinating ash and extracting potassium by cement kiln bypass air discharge |
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