CN103483456A - Preparation method of cement sizing fiber and application thereof in cement products - Google Patents
Preparation method of cement sizing fiber and application thereof in cement products Download PDFInfo
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- CN103483456A CN103483456A CN201310481390.4A CN201310481390A CN103483456A CN 103483456 A CN103483456 A CN 103483456A CN 201310481390 A CN201310481390 A CN 201310481390A CN 103483456 A CN103483456 A CN 103483456A
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Abstract
The invention discloses a preparation method of cement sizing fiber and an application thereof in cement products, belonging to the field of novel sizing fiber. The preparation method comprises the following steps: by taking plant raw material as raw material, firstly removing alcohol-soluble proteins, then alkalizing wheat bran in an alcohol solution to remove arabinoxylan by hydrolysis, further directly adding dichloromethane, performing etherification reaction, and linking the arabinoxylan which is removed by hydrolysis onto plant raw material fiber to prepare the cement sizing fiber; and the sizing fiber is used in cement, and the formula comprises 10-80% of cement, 20-80% of fine sand, 0-10% of additives and 0.5-20% of cement sizing fiber. The sizing fiber prepared by the preparation method disclosed by the invention is used in the cement and can significantly improve the compressive strength, the flexural strength and the leakage resistance of the cement.
Description
Technical field
The present invention relates to novel fiber sizing field, especially relate to a kind of preparation method of cement fiber sizing and the application in cement products thereof.
Background technology
Cement is current topmost material of construction, but the shortcoming such as sand-cement slurry and concrete exist that tensile strength is low, fragility is large and shock resistance is poor, fiber some alkali-resistivity is strong, good mechanical performance is mutually compound with cement products such as sand-cement slurry or concrete with different modes, can be in the mechanics that improves in varying degrees the latter and physicals, and improve their use value and weather resistance.The fortifying fibre used in engineering at present mainly contains glass fibre, synthetic organic fibre, and steel fiber etc., but all be limited by the high impact of price, and the weather resistance that glass fibre is used in cement is inadequate; Synthetic organic fibre mainly contains polypropylene fibre, and the interface binding power between this fiber and concrete is little, affects it and strengthen the performance of toughening effect in cement products; Steel fiber easily causes the problem of galvanic corrosion.
The mixed ether product processed by corn bran etc. can replace using timber, purified cotton, the derivative products such as starch, and polyvinyl alcohol, can disperse rubber powder, the petroleum chemicalss such as chemistry tamanori, China is global corn yield the second big country, 2009 annual production reach 1.6 hundred million tons, therefore, deeply develop the corn derived product, expand the corn product Application Areas, promote industrial chain and the technology thereof in corn processed field, Testa Tritici, brewer's grains, rice husk, Pericarppium arachidis hypogaeae, wheat straw, reed, timber etc. are generally also as refuse treatment, if can be as the Raw Material for Cement Production fiber sizing, also saved the energy, reach second stage employ.
Summary of the invention
Technical problem to be solved by this invention is: a kind of preparation method of cement fiber sizing and the application in cement products thereof are provided, take Testa Tritici, brewer's grains, rice husk, Pericarppium arachidis hypogaeae, wheat straw, reed, timber is raw material, through series of processes production, obtain, source is abundant, and it is of low nutritive value, therefore price is also cheap, excellent property.Due to sand-cement slurry and concrete consumption very big, market outlook are extremely wide.
For solving the problems of the technologies described above, technical scheme of the present invention is:
A kind of preparation method of cement fiber sizing, is characterized in that, comprises the following steps:
1. choose plant material,
2. plant material is removed to prolamine: in the Organic Alcohol aqueous solution, add 5～15% inorganic strong alkali, be warming up to 60～70 ℃, by its dissolving, then be cooled to 0～45 ℃;
3. the plant material that will 2. process through step is warming up to 60～100 ℃; Then be cooled to 0～45 ℃, add etherifying agent 45～95 ℃ of etherificates 4～12 hours, generate araboxylan methyl ether base ether of cellulose; Be cooled to 0～50 ℃, with organic acid, be neutralized to PH=6～9, filter, filter cake is used the Organic Alcohol solution washing again, and centrifugation can obtain cement fiber sizing product.
Preferably, 2. described step is: plant material is removed to prolamine: in the Organic Alcohol aqueous solution, add 5～15% inorganic strong alkali, be warming up to 65～70 ℃, by its dissolving, then be cooled to 0～45 ℃.
Preferably, 3. described step is: the plant material that will 2. process through step is warming up to 75～90 ℃; Then be cooled to 0～45 ℃, add etherifying agent 75～95 ℃ of etherificates 4～12 hours, generate araboxylan methyl ether base ether of cellulose; Be cooled to 0～50 ℃, with organic acid, be neutralized to PH=6～9, filter, the Organic Alcohol solution that filters out araboxylan methyl ether base ether of cellulose merges the Distillation recovery Organic Alcohol and recycles, filter cake is used the Organic Alcohol solution washing again, and centrifugation can obtain cement fiber sizing product.
Preferably, described plant material is: one or several of corn bran, Testa Tritici, brewer's grains, rice husk, Pericarppium arachidis hypogaeae, wheat straw, reed, timber;
Described step 2. middle Organic Alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, C4～C6 alcohol and isomery alcohol thereof, propylene glycol, glycerol, hexanaphthene, benzene, toluene;
Described step 2. middle inorganic strong alkali is sodium hydroxide, potassium hydroxide, sodium carbonate;
Described step 3. middle etherifying agent is: methylene dichloride, ethylene dichloride, propylene dichloride, dichlorobutane (C1～C16); Epoxy chloropropane;
Organic acid or the mineral acid of described step in 3. is hydrochloric acid, hydrogen chloride gas, sulfuric acid, phosphoric acid, formic acid, formic acid, acetic acid, oxyacetic acid, propionic acid.
Preferably, the proportioning in described Organic Alcohol alcohol solution is: Organic Alcohol: water=1: (0～2); The mass ratio of plant material and the Organic Alcohol aqueous solution is 1: (1～20); Plant material: inorganic strong alkali: the mass ratio of etherifying agent is 1:0.12～2.0: 0.2～0.3, and the weight of described plant material is the weight of having removed prolamine.
Preferably, the proportioning in described Organic Alcohol alcohol solution is: Organic Alcohol: water=1: (0.05～0.30); The mass ratio of plant material and the Organic Alcohol aqueous solution is 1: (5～12); Plant material: inorganic strong alkali: the mass ratio of etherifying agent is 1:0.2: 0.2, and the weight of described plant material is the weight of having removed prolamine.
Preferably, it is characterized in that only by plant material (having removed prolamine) alkalization hydrolysis, without etherification reaction, then directly neutralization is filtered, drying, can make araboxylan methyl ether base cellulose ether product, and the weight of described plant material is the weight of having removed prolamine.
The present invention also provides the application of a kind of cement fiber sizing in cement products, it is characterized in that, described cement products comprises the raw material of following weight ratio: cement 10～80%, aggregate 20～80%, additive 0～10%, cement fiber sizing 0.5～20%.
Preferably, described cement is one or several in silicate cement, high-alumina cement, lime cement, high phosphorus cement, portland blast-furnace slag cement.
Preferably, described aggregate is one or several in fine sand, amorphous silicon oxide, SILICA FUME, diatomite, coal ash and bottom ash, rice hull ash, blast furnace slag, grain slag, scum, clay, magnesite, rhombspar, metal oxide or oxyhydroxide, resin particle.
Adopted technique scheme, beneficial effect of the present invention is:
The fiber sizing of patented invention is to take plant as raw material, through series of processes production, obtains, and source is abundant, and it is of low nutritive value, therefore price is also cheap, and excellent property.Due to sand-cement slurry and concrete consumption very big, market outlook are extremely wide.
The present invention is significant to the deep processing that promotes agricultural planting industry and agricultural planting simultaneously, for it has opened up a new cycle applications field, and environmental protection, benefit is obvious.
The standby fiber sizing of patent system of the present invention is used for cement, can significantly improve ultimate compression strength, folding strength and the impermeability of cement.
Embodiment
Below in conjunction with embodiment, the present invention is further described.
Example 1
In the 10L autoclave pressure, add the 5.0L90% aqueous ethanolic solution, add 99% sodium hydroxide 50.5g, be heated to 60～70 ℃, by dissolution of sodium hydroxide or dispersion aqueous ethanolic solution, dissolution time 1 hour; Cool to 0～45 ℃, then add corn bran (removing prolamine) 500g, be warming up to 60～100 ℃, hydrolysis alkalization 0.5～4 hour; Be cooled to 0～45 ℃, add 98% ethylene dichloride 37.5g, be warming up to 45～95 ℃, etherificate 4～12 hours; Etherificate is cooled to 0～45 ℃ after finishing, and adds 95% acetic acid and is neutralized to PH=6～9; Centrifugation, 10L60% aqueous ethanolic solution continuous washing secondary for filter cake, dry under 80 ℃ of filter cakes, the araboxylan methyl ether base cellulose ether product that to obtain purity be 98%.
Example 2
Identical with example 1, corn bran is changed into to Testa Tritici.
Example 3
Identical with example 1, change the mixture of corn bran and Testa Tritici into, weight ratio is 1: 1.
Example 4
In the 10L autoclave pressure, add the 5.0L90% aqueous ethanolic solution, add 99% sodium hydroxide 50.5g, be heated to 60～70 ℃, by dissolution of sodium hydroxide or dispersion aqueous ethanolic solution, dissolution time 1 hour; Cool to 0～45 ℃, then add corn bran (removing prolamine) 500g, be warming up to 60～100 ℃, hydrolysis alkalization 0.5～4 hour; Be cooled to 0～45 ℃, add 95% acetic acid and be neutralized to PH=6～9; Centrifugation, 10L60% aqueous ethanolic solution continuous washing secondary for filter cake, dry under 80 ℃ of filter cakes, obtain low molecular mixing ether fiber sizing.
Example 5
The fiber sizing made by example 1 is applied in the actual production of cement products.
The formula of cement products sample is: 10% fiber sizing, 10% calcium silicate hydrate (weightening finish filler), 0.15% methylcellulose gum (thickening material), 39.25% silicate cement, 39.25% fine sand.
Do not add fiber sizing in control sample.
At room temperature natural drying maintenance of sample sclerosis 28 days, then carry out the physical and mechanical properties test.Carry out resistance to compression and folding strength test by GB/T50081-2002, by GB/T50082-2009, carry out Standard Test Method for Permeation Resistance, result is as shown in table 1 below.
Add fiber sizing in table 1 the present embodiment and do not add the physical and mechanical properties test chart of fiber sizing
| Physicals | A | The B(control sample) |
| Ultimate compression strength (MPa) | 39.1 | 36.7 |
| Folding strength (MPa) | 5.1 | 4.2 |
| Impervious (cm) | 8.5 | 14 |
From upper table 1, fiber sizing can improve physical and mechanical properties and the weather resistance of cement products greatly.
Example 6
The fiber sizing made by example 4 is applied in the actual production of cement products.
The formula of cement products sample is: 10% fiber sizing, 10% calcium silicate hydrate (weightening finish filler), 0.15% methylcellulose gum (thickening material), 39.25% silicate cement, 39.25% fine sand.
Do not add fiber sizing in control sample.
At room temperature natural drying maintenance of sample sclerosis 28 days, then carry out the physical and mechanical properties test.Carry out resistance to compression and folding strength test by GB/T50081-2002, by GB/T50082-2009, carry out Standard Test Method for Permeation Resistance.
Add fiber sizing in table 2 the present embodiment and do not add the physical and mechanical properties test chart of fiber sizing
| Physicals | A | The B(control sample) |
| Ultimate compression strength (MPa) | 38.4 | 36.7 |
| Folding strength (MPa) | 4.9 | 4.2 |
| Impervious (cm) | 7.5 | 14 |
As seen from the above table, also can greatly improve physical and mechanical properties and the weather resistance of cement products by the fiber sizing of simplifying explained hereafter.
The present invention is not limited to above-mentioned concrete embodiment, and those of ordinary skill in the art is from above-mentioned design, and without performing creative labour, all conversion of having done, within all dropping on protection scope of the present invention.
Claims (10)
1. the preparation method of a cement fiber sizing, is characterized in that, comprises the following steps:
1. choose plant material;
2. plant material is removed to prolamine: in the Organic Alcohol aqueous solution, add 5～15% inorganic strong alkali, be warming up to 60～70 ℃, by its dissolving, then be cooled to 0～45 ℃;
3. the plant material that will 2. process through step is warming up to 60～100 ℃; Then be cooled to 0～45 ℃, add etherifying agent 45～95 ℃ of etherificates 4～12 hours, generate araboxylan methyl ether base ether of cellulose; Be cooled to 0～50 ℃, with organic acid, be neutralized to PH=6～9, filter, filter cake is used the Organic Alcohol solution washing again, and centrifugation can obtain cement fiber sizing product.
2. preparation method according to claim 1, is characterized in that, 2. described step is: plant material is removed to prolamine: in the Organic Alcohol aqueous solution, add 5～15% inorganic strong alkali, be warming up to 65～70 ℃, by its dissolving, then be cooled to 0～45 ℃.
3. preparation method according to claim 1, is characterized in that, 3. described step is: the plant material that will 2. process through step is warming up to 75～90 ℃; Then be cooled to 0～45 ℃, add etherifying agent 75～95 ℃ of etherificates 4～12 hours, generate araboxylan methyl ether base ether of cellulose; Be cooled to 0～50 ℃, with organic acid, be neutralized to PH=6～9, filter, the Organic Alcohol solution that filters out araboxylan methyl ether base ether of cellulose merges the Distillation recovery Organic Alcohol and recycles, filter cake is used the Organic Alcohol solution washing again, and centrifugation can obtain cement fiber sizing product.
4. preparation method according to claim 1, is characterized in that, described plant material is: one or several of corn bran, Testa Tritici, brewer's grains, rice husk, Pericarppium arachidis hypogaeae, wheat straw, reed, timber;
Described step 2. middle Organic Alcohol is methyl alcohol, ethanol, propyl alcohol, Virahol, C4～C6 alcohol and isomery alcohol thereof, propylene glycol, glycerol, hexanaphthene, benzene, toluene;
Described step 2. middle inorganic strong alkali is sodium hydroxide, potassium hydroxide, sodium carbonate;
Described step 3. middle etherifying agent is: methylene dichloride, ethylene dichloride, propylene dichloride, dichlorobutane (C1～C16); Epoxy chloropropane;
Organic acid or the mineral acid of described step in 3. is hydrochloric acid, hydrogen chloride gas, sulfuric acid, phosphoric acid, formic acid, formic acid, acetic acid, oxyacetic acid, propionic acid.
5. preparation method according to claim 1, is characterized in that, the proportioning in described Organic Alcohol alcohol solution is: Organic Alcohol: water=1: (0～2); The mass ratio of plant material and the Organic Alcohol aqueous solution is 1: (1～20); Plant material: inorganic strong alkali: the mass ratio of etherifying agent is 1:0.12～2.0: 0.2～0.3, and the weight of described plant material is the weight of having removed prolamine.
6. preparation method according to claim 5, is characterized in that, the proportioning in described Organic Alcohol alcohol solution is: Organic Alcohol: water=1: (0.05～0.30); The mass ratio of plant material and the Organic Alcohol aqueous solution is 1: (5～12); Plant material: inorganic strong alkali: the mass ratio of etherifying agent is 1:0.2: 0.2, and the weight of described plant material is the weight of having removed prolamine.
7. preparation method according to claim 1, it is characterized in that only by plant material (having removed prolamine) alkalization hydrolysis, without etherification reaction, then directly neutralization is filtered, dry, can make araboxylan methyl ether base cellulose ether product, the weight of described plant material is the weight of having removed prolamine.
8. the application of cement fiber sizing in cement products, is characterized in that, described cement products comprises the raw material of following weight ratio: cement 10～80%, aggregate 20～80%, additive 0～10%, cement fiber sizing 0.5～20%.
9. the application of a kind of cement fiber sizing according to claim 8 in cement products, is characterized in that, described cement is one or several in silicate cement, high-alumina cement, lime cement, high phosphorus cement, portland blast-furnace slag cement.
10. the application of a kind of cement fiber sizing according to claim 8 in cement, it is characterized in that, described aggregate is one or several in fine sand, amorphous silicon oxide, SILICA FUME, diatomite, coal ash and bottom ash, rice hull ash, blast furnace slag, grain slag, scum, clay, magnesite, rhombspar, metal oxide or oxyhydroxide, resin particle.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107476104A (en) * | 2017-08-11 | 2017-12-15 | 广东龙湖科技股份有限公司 | A kind of preparation method and its product with hydrophobic function wood fibre |
| CN108149999A (en) * | 2016-12-03 | 2018-06-12 | 王士勇 | A kind of novel combined electric pole |
| US20220033304A1 (en) * | 2020-07-29 | 2022-02-03 | University Of Louisville Research Foundation, Inc. | Biomass waste materials as a set-retardation agent in cement or concrete |
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| US20010020091A1 (en) * | 1999-02-10 | 2001-09-06 | Eastman Chemical Company | Corn fiber for the production of advanced chemicals and materials: arabinoxylan and arabinoxylan derivatives prepared therefrom |
| CN1844026A (en) * | 2006-04-21 | 2006-10-11 | 华南理工大学 | A novel masonry cement |
| CN101182139A (en) * | 2007-11-12 | 2008-05-21 | 华南理工大学 | Masonry cement having higher strength and water retention |
| CN102718874A (en) * | 2012-06-29 | 2012-10-10 | 新乡市东升新材料有限公司 | Method for preparing methyl cellulose ether with arundodomax dissolving pulp serving as raw material |
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2013
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20010020091A1 (en) * | 1999-02-10 | 2001-09-06 | Eastman Chemical Company | Corn fiber for the production of advanced chemicals and materials: arabinoxylan and arabinoxylan derivatives prepared therefrom |
| CN1844026A (en) * | 2006-04-21 | 2006-10-11 | 华南理工大学 | A novel masonry cement |
| CN101182139A (en) * | 2007-11-12 | 2008-05-21 | 华南理工大学 | Masonry cement having higher strength and water retention |
| CN102718874A (en) * | 2012-06-29 | 2012-10-10 | 新乡市东升新材料有限公司 | Method for preparing methyl cellulose ether with arundodomax dissolving pulp serving as raw material |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108149999A (en) * | 2016-12-03 | 2018-06-12 | 王士勇 | A kind of novel combined electric pole |
| CN107476104A (en) * | 2017-08-11 | 2017-12-15 | 广东龙湖科技股份有限公司 | A kind of preparation method and its product with hydrophobic function wood fibre |
| US20220033304A1 (en) * | 2020-07-29 | 2022-02-03 | University Of Louisville Research Foundation, Inc. | Biomass waste materials as a set-retardation agent in cement or concrete |
| US11851371B2 (en) * | 2020-07-29 | 2023-12-26 | University Of Louisville Research Foundation, Inc. | Biomass waste materials as a set-retardation agent in cement or concrete |
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Effective date of registration: 20190708 Address after: 518052 Room 201, building A, No. 1, Qian Wan Road, Qianhai Shenzhen Hong Kong cooperation zone, Shenzhen, Guangdong (Shenzhen Qianhai business secretary Co., Ltd.) Patentee after: Shenzhen Mo Dun environmental protection new material Co., Ltd. Address before: No. 168 Airway Road, Liuhe Industrial Park, Xiaogan City, Hubei Province, 432000 Patentee before: Hubei Professional New Biological Material Co., Ltd. |