CN102875049B - High sulfonation degree aliphatic water reducing agent and preparation method thereof - Google Patents
High sulfonation degree aliphatic water reducing agent and preparation method thereof Download PDFInfo
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- CN102875049B CN102875049B CN201210428354.7A CN201210428354A CN102875049B CN 102875049 B CN102875049 B CN 102875049B CN 201210428354 A CN201210428354 A CN 201210428354A CN 102875049 B CN102875049 B CN 102875049B
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Abstract
The invention discloses a high sulfonation degree aliphatic water reducing agent and a preparation method of the high sulfonation degree aliphatic water reducing agent. The water reducing agent is prepared by pyrosulfite, ketone compounds, aldehydes compounds, lignosulfonate, water and caustic soda liquid. The preparation method comprises the following steps of: adding the weighed water, pyrosulfite, caustic soda liquid and lignosulfonate to a reacting container, and uniformly agitating; then adding 1 to 5 parts of aldehydes compounds to react for 1 to 2 hours; then synchronously dropping ketone compounds, and the rest aldehydes compounds for 1 to 3 hours; and finally keeping the temperature for 1 to 3 hours at 80 to 95 DEG C. With the adoption of the high sulfonation degree aliphatic water reducing agent and the preparation method disclosed by the invention, producing cost is effectively reduced; compared with a traditional technology of sulfonating acetone first, the method adopting sulfonating formaldehyde first can effectively improve a sulfonation degree, and more water reducing groups are introduced, therefore, the synthesized aliphatic water reducing agent has a higher effect on water reducing. With the adoption of the preparation method disclosed by the invention for producing the water reducing agent, operation is simple and convenient to carry out, and a production period is short.
Description
Technical field
The present invention relates to cement water reducing agent field, particularly relate to a kind of highly sulfonated aliphatic water reducing agent and preparation method thereof.
Background technology
High efficiency water reducing agent is one of main raw material of producing high-strength, high performance concrete.At home on market, the high efficiency water reducing agent of use mainly contains naphthalene water reducer, sulfonated melamine based water reducer, sulfamate based water reducer and polycarboxylate based water reducer at present.Wherein naphthalene water reducer usage quantity maximum, but it exists some defects: such as environmental pollution in production process is more serious; Water-reducing rate is not very high; Product function of slump protection is poor; Sodium sulphate content is high, has the phenomenon of crystalline deposit winter.And the price volalility of primary industry naphthalene is larger.
Aliphatic water reducing agent is the novel water reducer of one growing up the eighties in last century.It is taking acetone, formaldehyde, sulphite etc. as main raw material, through oversulfonate, condensation and the anionic polymer tensio-active agent making.Aliphatic water reducing agent has that volume is low, sodium sulphate content is few (being less than 1%), winter is without crystallization, to features such as reinforcing bar non-corrodings, belongs to early strong non-research work of air entrained type water reducer, applies at present more in high-strength pipe pile is produced.But, along with the price of sulphite rises steadily, also increased the cost of aliphatic water reducing agent, in addition, but the traditional technology of aliphatic water reducing agent adopts the technique of earlier sulfonation acetone, and sulfonation degree is inadequate, has limited the introducing of diminishing group, its water-reducing effect is only omited height a bit with respect to naphthalene water reducer, does not reach the effect of high diminishing.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of production cost that can effectively reduce water reducer, can effectively improve sulfonation degree, introduce more diminishing group, make synthetic aliphatic water reducing agent there is highly sulfonated aliphatic water reducing agent of higher water-reducing effect and preparation method thereof.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: a kind of highly sulfonated aliphatic water reducing agent is provided, be prepared from by pyrosulfite, ketone compounds, aldehyde compound, sulfonated lignin, water and liquid caustic soda, the parts by weight of each raw material are: 1 ~ 10 part of 6 ~ 15 parts of pyrosulfites, 3 ~ 6 parts of ketone compounds, 10 ~ 35 parts of aldehyde compounds, 1 ~ 3 part of sulfonated lignin, 20 ~ 46 parts, water and liquid caustic soda.
In a preferred embodiment of the present invention, described pyrosulfite is Sodium Pyrosulfite or potassium pyrosulfite.
In a preferred embodiment of the present invention, described ketone compounds is acetone, pentanone, pimelinketone, methylethylketone or diacetylmethane.
In a preferred embodiment of the present invention, described aldehyde compound is formaldehyde, acetaldehyde, Metaldehyde, phenylpropionaldehyde or hexanal.
In a preferred embodiment of the present invention, described sulfonated lignin are sodium lignosulfonate or calcium lignin sulphonate.
For solving the problems of the technologies described above, another technical solution used in the present invention is: a kind of preparation method of highly sulfonated aliphatic water reducing agent is provided, comprises the steps:
First take each raw material according to parts by weight; The water taking, pyrosulfite, liquid caustic soda, sulfonated lignin are added in reaction vessel, stir, then add the aldehyde compound of 1 ~ 5 part, under 30 ~ 45 DEG C of conditions, react 1 ~ 2 hour; Then drip ketone compounds and remaining aldehyde compound simultaneously, control rate of addition, dropwise with 1 ~ 3 h, finally at 80 ~ 95 DEG C, be incubated 1 ~ 3 hour, can make highly sulfonated aliphatic water reducing agent.
The invention has the beneficial effects as follows: the present invention has used low-cost pyrosulfite and sulfonated lignin, effectively reduce the production cost of water reducer, and the present invention adopts the method for earlier sulfonation formaldehyde, with the technique of traditional earlier sulfonation acetone by comparison, can effectively improve sulfonation degree, introduce more diminishing group, make synthetic aliphatic water reducing agent there is higher water-reducing effect.The present invention adopts this explained hereafter water reducer easy and simple to handle, with short production cycle.
Embodiment
Below preferred embodiment of the present invention is described in detail, thereby so that advantages and features of the invention can be easier to be it will be appreciated by those skilled in the art that, protection scope of the present invention is made to more explicit defining.
Embodiment 1
A kind of highly sulfonated aliphatic water reducing agent, preparation by the following method, concrete steps are as follows:
First take each raw material according to parts by weight; 2 parts, 32 parts, the water taking, 11 parts of Sodium Pyrosulfites, 5 parts of liquid caustic soda, calcium lignin sulphonate is added in reaction vessel, stir, then add 15 parts, formaldehyde, under 38 DEG C of conditions, react 2 hours; Then drip 5 parts, 4 parts, acetone and remaining formaldehyde simultaneously, control rate of addition, dropwise with 2 h, finally at 80 DEG C, be incubated 3 hours, can make highly sulfonated aliphatic water reducing agent.
Embodiment 2
A kind of highly sulfonated aliphatic water reducing agent, preparation by the following method, concrete steps are as follows:
First take each raw material according to parts by weight; 3 parts, 20 parts, the water taking, 6 parts of Sodium Pyrosulfites, 1 part of liquid caustic soda, calcium lignin sulphonate is added in reaction vessel, stir, then add 8 parts, formaldehyde, under 30 DEG C of conditions, react 1 hour; Then drip 2 parts, 3 parts, acetone and remaining formaldehyde simultaneously, control rate of addition, dropwise with 1 h, finally at 87 DEG C, be incubated 2 hours, can make highly sulfonated aliphatic water reducing agent.
Embodiment 3
A kind of highly sulfonated aliphatic water reducing agent, preparation by the following method, concrete steps are as follows:
First take each raw material according to parts by weight; 3 parts, 46 parts, the water taking, 15 parts of Sodium Pyrosulfites, 10 parts of liquid caustic soda, sodium lignosulfonate is added in reaction vessel, stir, then add 28 parts, formaldehyde, under 38 DEG C of conditions, react 2 hours; Then drip 7 parts, 6 parts, acetone and remaining formaldehyde simultaneously, control rate of addition, dropwise with 3 h, finally at 95 DEG C, be incubated 1 hour, can make highly sulfonated aliphatic water reducing agent.
The present invention has used low-cost pyrosulfite and sulfonated lignin, effectively reduce the production cost of water reducer, and the present invention adopts the method for earlier sulfonation formaldehyde, with the technique of traditional earlier sulfonation acetone by comparison, can effectively improve sulfonation degree, introduce more diminishing group, make synthetic aliphatic water reducing agent there is higher water-reducing effect.The present invention adopts this explained hereafter water reducer easy and simple to handle, with short production cycle.
The foregoing is only embodiments of the invention; not thereby limit the scope of the claims of the present invention; every equivalent structure or conversion of equivalent flow process that utilizes specification sheets of the present invention to do, or be directly or indirectly used in other relevant technical fields, be all in like manner included in scope of patent protection of the present invention.
Claims (5)
1. a highly sulfonated aliphatic water reducing agent, it is characterized in that, be prepared from by pyrosulfite, ketone compounds, aldehyde compound, sulfonated lignin, water and liquid caustic soda, the parts by weight of each raw material are: 1 ~ 10 part of 6 ~ 15 parts of pyrosulfites, 3 ~ 6 parts of ketone compounds, 10 ~ 35 parts of aldehyde compounds, 1 ~ 3 part of sulfonated lignin, 20 ~ 46 parts, water and liquid caustic soda;
Its preparation method, comprises the steps:
First take each raw material according to parts by weight; The water taking, pyrosulfite, liquid caustic soda, sulfonated lignin are added in reaction vessel, stir, then add the aldehyde compound of 1 ~ 5 part, under 30 ~ 45 DEG C of conditions, react 1 ~ 2 hour; Then drip ketone compounds and remaining aldehyde compound simultaneously, control rate of addition, dropwise with 1 ~ 3 h, finally at 80 ~ 95 DEG C, be incubated 1 ~ 3 hour, can make highly sulfonated aliphatic water reducing agent.
2. highly sulfonated aliphatic water reducing agent according to claim 1, is characterized in that, described pyrosulfite is Sodium Pyrosulfite or potassium pyrosulfite.
3. highly sulfonated aliphatic water reducing agent according to claim 1, is characterized in that, described ketone compounds is acetone, pentanone, pimelinketone, methylethylketone or diacetylmethane.
4. highly sulfonated aliphatic water reducing agent according to claim 1, is characterized in that, described aldehyde compound is formaldehyde, acetaldehyde, Metaldehyde, phenylpropionaldehyde or hexanal.
5. highly sulfonated aliphatic water reducing agent according to claim 1, is characterized in that, described sulfonated lignin are sodium lignosulfonate or calcium lignin sulphonate.
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| CN104478280B (en) * | 2014-12-30 | 2017-02-01 | 福建清源科技有限公司 | Concrete synergist and preparation method thereof |
| CN106396456B (en) * | 2016-08-26 | 2018-07-03 | 河南科之杰新材料有限公司 | A kind of preparation method of aliphatic powder water-reducing agent |
| CN108046640B (en) * | 2017-12-19 | 2020-11-27 | 萧县沃德化工科技有限公司 | Aliphatic superplasticizer modified by 2-naphthol waste liquid and preparation method thereof |
| CN109553326A (en) * | 2018-11-24 | 2019-04-02 | 南京福盛建材有限公司 | A kind of high-thin arch dam aliphatic water reducing agent and preparation method thereof |
| CN111056760B (en) * | 2019-12-21 | 2022-05-20 | 浙江吉盛化学建材有限公司 | Aliphatic water reducer prepared from aminobenzenesulfonic acid wastewater and synthesis process thereof |
| CN113248177A (en) * | 2021-07-06 | 2021-08-13 | 四川宇砼建材有限公司 | High-performance composite water reducing agent and preparation method thereof |
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| CN101665337A (en) * | 2009-09-03 | 2010-03-10 | 南京林业大学 | Modified aliphatic high-efficiency water-reducing agent by utilizing lignosulfonate and preparation method thereof |
| CN101870566A (en) * | 2010-06-23 | 2010-10-27 | 江苏汇迪建材有限公司 | Alkali lignin modified aliphatic high efficiency water reducing agent and preparation method thereof |
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