CN108609886A - The method that the spent lye of mercerization prepares aliphatic water reducing agent - Google Patents
The method that the spent lye of mercerization prepares aliphatic water reducing agent Download PDFInfo
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- CN108609886A CN108609886A CN201810482486.5A CN201810482486A CN108609886A CN 108609886 A CN108609886 A CN 108609886A CN 201810482486 A CN201810482486 A CN 201810482486A CN 108609886 A CN108609886 A CN 108609886A
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- parts
- reducing agent
- water reducing
- spent lye
- aliphatic water
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The present invention relates to aliphatic water reducing agent preparation and environmental protection technical fields; more particularly to a kind of method that the spent lye of mercerization prepares aliphatic water reducing agent; utilize the obtained aliphatic water reducing agents such as fiber, dyestuff, bleeding agent in spent lye; the building-up process of aliphatic water reducing agent is catalyzed using the sodium hydroxide in spent lye simultaneously; increase condensation reaction activity; reaction speed is improved, the aliphatic water reducing agent is prepared by the raw material of following parts by weight：150 300 parts of water, 60 100 parts of sodium nitrite, 60 100 parts of sodium pyrosulfite, 230 280 parts of formalin, 100 200 parts of spent lye, 95 110 parts of acetone.The present invention directly utilizes the spent lye generated in mercerization processing procedure; at low cost, slump is prepared and keeps the aliphatic water reducing agent that effect is good, water-reducing rate is high; solves salkali waste liquid recovering and process technology complexity, processing is not thorough, consumes energy the problems such as big, of high cost; improve the utilization rate of hazardous waste; environmental protection, remarkable in economical benefits.
Description
Technical field
The present invention relates to aliphatic water reducing agent preparation and environmental protection technical fields, and in particular to a kind of mercerization gives up
The method that lye prepares aliphatic water reducing agent.
Background technology
Mercerization is to be handled the yarn and fabric of pure cotton or high cotton content to increase it with sodium hydroxide solution
The technique of lustrous surface.The mercerized waste alkali generated in the process (usually contains the hydroxide of 10-35% or so in strong basicity
Sodium), wherein coloration, COD and ss suspended solid value are higher, and impurity component is more, including fiber, dyestuff, chemical sizwe, infiltration
Agent, fluorescent whitening agent and inorganic salts etc. are directly discharged not only waste of resource if not recycled, but also can be to environment
Larger pollution is caused, hazardous waste is belonged to.If the spent lye that industry generates mostly uses acid solution greatly without recycling and is carried out to it
It is discharged after neutralisation treatment, wastes a large amount of acid solution, cause secondary pollution, and largely waste the various composition in spent lye, institute
To be recycled spent lye as inexorable trend.It is de- that the spent lye generated during mercerization finish commonly uses oxidation at present
Color, separating-purifying mode handled, not only processing is complicated, energy consumption is big, increases operation cost, and processing is not thorough.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of spent lyes of mercerization to prepare aliphatic water reducing agent
Method improves the utilization rate for the spent lye that mercerization generates, and at low cost, slump is prepared and keeps that effect is good, water-reducing rate
High aliphatic water reducing agent reduces the difficulty of salkali waste liquid recovering and process technology, saves energy consumption.
In order to achieve the above object, the present invention is achieved by the following technical programs：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(1) it adds water in four-hole boiling flask, sodium nitrite and sodium pyrosulfite is added under stirring, be stirred
After even, the pH value that spent lye is added to mixed system is 7-9, continues to be stirred to react 30min；
(2) acetone is weighed in constant pressure funnel, being added dropwise acetone into the product of step (1), time for adding 20-30min,
It is stirred to react 30min after being added dropwise, continues that formalin, time for adding 1.5-2h, by reactant after being added dropwise is added dropwise
System is heated to 95 DEG C, and heat preservation is cooled to room temperature after heat preservation, obtains aliphatic water reducing agent.
Further, the aliphatic water reducing agent is prepared by the raw material of following parts by weight：150-300 parts of water, nitrous
Sour sodium 60-100 parts, 60-100 parts of sodium pyrosulfite, 230-280 parts of formalin, 100-200 parts of spent lye, acetone 95-110
Part.
Further, the purity of the sodium nitrite is 80%.
Further, the aliphatic water reducing agent is prepared by the raw material of following parts by weight：280-300 parts of water, nitrous
Sour sodium 80-95 parts, 80-95 parts of sodium pyrosulfite, 265-275 parts of formalin, 190-200 parts of spent lye, acetone 105-110
Part.
Further, the aliphatic water reducing agent is prepared by the raw material of following parts by weight：290 parts of water, sodium nitrite
95 parts, 90 parts of sodium pyrosulfite, 270 parts of formalin, 200 parts of spent lye, 105 parts of acetone.
Further, the soaking time of the step (2) is 2-4h.
Further, a concentration of the 37% of the formalin.
Due to using above-mentioned technical solution, of the invention is beneficial as follows：
(1) present invention is directly using the spent lye generated in mercerization processing procedure, without directly being used through any processing
In preparing modified aliphatic high efficiency water reducing agent, pollution of the waste discharge to environment is avoided, solves spent lye recovery processing work
Skill is complicated, processing is not thorough, consumes energy the problems such as big, of high cost, improves the utilization rate for the hazardous waste that mercerization generates, protection
Environment, remarkable in economical benefits；
(2) present invention introduces spent lye in fiber, the hydroxyl in dyestuff, phenolic hydroxyl group, carbonyl etc. can participate in gathering
It closes, can be grafted with aliphatic compound, increase the branch quantity in aliphatic water reducing agent in condensation course, improve concrete
Slump effect, while the sodium hydroxide in spent lye is catalyzed the building-up process of modified aliphatic water reducing agent, increases contracting
The activity of reaction is closed, reaction speed is improved；
(3) in mercerization finish spent lye used in the present invention other impurity on water-reducing agent color, quality without influence, it is right
Environmental nonpollution.
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 kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(3) 290 parts of water is added in four-hole boiling flask, the nitrous acid that the purity that 95 parts are added under stirring is 80%
The sodium pyrosulfite of sodium and 90 parts of technical grade, after being uniformly mixed, be added 200 parts spent lye to mixed system pH value
It is 8, continues to be stirred to react 30min；
(4) acetone for weighing 105 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
30min is stirred to react 30min after being added dropwise, and continues that 270 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 3.5h is cooled to room temperature, i.e., after heat preservation
Aliphatic water reducing agent is made.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 2：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(5) 280 parts of water is added in four-hole boiling flask, the nitrous acid that the purity that 80 parts are added under stirring is 80%
The sodium pyrosulfite of sodium and 80 parts of technical grade, after being uniformly mixed, be added 190 parts spent lye to mixed system pH value
It is 8, continues to be stirred to react 30min；
(6) acetone for weighing 105 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
25min is stirred to react 30min after being added dropwise, and continues that 265 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 4h is cooled to room temperature after heat preservation, that is, makes
Obtain aliphatic water reducing agent.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 3：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(7) 300 parts of water is added in four-hole boiling flask, the nitrous acid that the purity that 95 parts are added under stirring is 80%
The sodium pyrosulfite of sodium and 95 parts of technical grade, after being uniformly mixed, be added 200 parts spent lye to mixed system pH value
It is 8, continues to be stirred to react 30min；
(8) acetone for weighing 110 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
30min is stirred to react 30min after being added dropwise, and continues that 275 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 3h is cooled to room temperature after heat preservation, that is, makes
Obtain aliphatic water reducing agent.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 4：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(9) 280 parts of water is added in four-hole boiling flask, the nitrous acid that the purity that 95 parts are added under stirring is 80%
The sodium pyrosulfite of sodium and 95 parts of technical grade, after being uniformly mixed, be added 190 parts spent lye to mixed system pH value
It is 8, continues to be stirred to react 30min；
(10) acetone for weighing 105 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
20min is stirred to react 30min after being added dropwise, and continues that 275 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 2h is cooled to room temperature after heat preservation, that is, makes
Obtain aliphatic water reducing agent.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 5：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(11) 150 parts of water is added in four-hole boiling flask, the nitrous that the purity that 60 parts are added under stirring is 80%
The sodium pyrosulfite of sour sodium and 60 parts of technical grade, after being uniformly mixed, be added 100 parts spent lye to mixed system pH
Value is 8, continues to be stirred to react 30min；
(12) acetone for weighing 95 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
20min is stirred to react 30min after being added dropwise, and continues that 230 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 1.5h after being added dropwise, and heat preservation, soaking time 3h is cooled to room temperature, i.e., after heat preservation
Aliphatic water reducing agent is made.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 6：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(13) 300 parts of water is added in four-hole boiling flask, the nitrous that the purity that 100 parts are added under stirring is 80%
After being uniformly mixed, 200 parts of spent lye is added to mixed system in the sodium pyrosulfite of sour sodium and 100 parts of technical grade
PH value is 8, continues to be stirred to react 30min；
(14) acetone for weighing 110 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
30min is stirred to react 30min after being added dropwise, and continues that 280 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 4h is cooled to room temperature after heat preservation, that is, makes
Obtain aliphatic water reducing agent.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 7：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(15) 150 parts of water is added in four-hole boiling flask, the nitrous that the purity that 60 parts are added under stirring is 80%
The sodium pyrosulfite of sour sodium and 60 parts of technical grade, after being uniformly mixed, be added 200 parts spent lye to mixed system pH
Value is 9, continues to be stirred to react 30min；
(16) acetone for weighing 95 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
20min is stirred to react 30min after being added dropwise, and continues that 230 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 1.5h after being added dropwise, and heat preservation, soaking time 3h is cooled to room temperature, i.e., after heat preservation
Aliphatic water reducing agent is made.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
Embodiment 8：
A kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, includes the following steps：
(17) 300 parts of water is added in four-hole boiling flask, the nitrous that the purity that 100 parts are added under stirring is 80%
After being uniformly mixed, 100 parts of spent lye is added to mixed system in the sodium pyrosulfite of sour sodium and 100 parts of technical grade
PH value is 7, continues to be stirred to react 30min；
(18) acetone for weighing 110 parts acetone is added dropwise into the product of step (1), time for adding is in constant pressure funnel
30min is stirred to react 30min after being added dropwise, and continues that 280 parts of a concentration of 37% formalin is added dropwise, time for adding is
Reaction system is heated to 95 DEG C by 2h after being added dropwise, and heat preservation, soaking time 4h is cooled to room temperature after heat preservation, that is, makes
Obtain aliphatic water reducing agent.
Obtained aliphatic water reducing agent is added in concrete mix as an aqueous solution, and volume is cement weight
0.8-3.0%.
Raw material：
To commonly use aliphatic water reducing agent as a control group in the market, the aliphatic diminishing with 1-8 preparations of the embodiment of the present invention
Agent is added in concrete mix as an aqueous solution, and volume is the 1.6% of cement weight, performance comparison data such as 1 institute of table
Show：
1 water-reducing rate of table and slump
By the result of table 1 as it can be seen that 1-8 products of the embodiment of the present invention are added in concrete mix, water-reducing rate and slump
Degree parameter is superior to control group.
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 (7)
1. a kind of method that the spent lye of mercerization prepares aliphatic water reducing agent, which is characterized in that include the following steps：
(1) it adds water in four-hole boiling flask, sodium nitrite and sodium pyrosulfite is added under stirring, is uniformly mixed
Afterwards, the pH value that spent lye is added to mixed system is 7-9, continues to be stirred to react 30min；
(2) acetone is weighed in constant pressure funnel, being added dropwise acetone into the product of step (1), and time for adding 20-30min is added dropwise
After be stirred to react 30min, continue that formalin is added dropwise, time for adding 1.5-2h adds reaction system after being added dropwise
To 95 DEG C, heat preservation is cooled to room temperature after heat preservation, obtains aliphatic water reducing agent heat.
2. the method that the spent lye of mercerization as described in claim 1 prepares aliphatic water reducing agent, which is characterized in that described
Aliphatic water reducing agent is prepared by the raw material of following parts by weight：150-300 parts of water, 60-100 parts of sodium nitrite, pyrosulfurous acid
60-100 parts of sodium, 230-280 parts of formalin, 100-200 parts of spent lye, 95-110 parts of acetone.
3. the method that the spent lye of mercerization as claimed in claim 1 or 2 prepares aliphatic water reducing agent, which is characterized in that
The purity of the sodium nitrite is 80%.
4. the method that the spent lye of mercerization as claimed in claim 2 prepares aliphatic water reducing agent, which is characterized in that described
Aliphatic water reducing agent is prepared by the raw material of following parts by weight：280-300 parts of water, 80-95 parts of sodium nitrite, sodium pyrosulfite
80-95 parts, 265-275 parts of formalin, 190-200 parts of spent lye, 105-110 parts of acetone.
5. the method that the spent lye of mercerization as claimed in claim 4 prepares aliphatic water reducing agent, which is characterized in that described
Aliphatic water reducing agent is prepared by the raw material of following parts by weight：290 parts of water, 95 parts of sodium nitrite, 90 parts of sodium pyrosulfite, first
270 parts of aldehyde solution, 200 parts of spent lye, 105 parts of acetone.
6. the method that the spent lye of mercerization as described in claim 1 prepares aliphatic water reducing agent, which is characterized in that described
The soaking time of step (2) is 2-4h.
7. the method that the spent lye of mercerization as described in claim 1 prepares aliphatic water reducing agent, which is characterized in that described
A concentration of the 37% of formalin.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810482486.5A CN108609886A (en) | 2018-05-18 | 2018-05-18 | The method that the spent lye of mercerization prepares aliphatic water reducing agent |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810482486.5A CN108609886A (en) | 2018-05-18 | 2018-05-18 | The method that the spent lye of mercerization prepares aliphatic water reducing agent |
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| CN108609886A true CN108609886A (en) | 2018-10-02 |
Family
ID=63663423
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234865A (en) * | 2007-08-22 | 2008-08-06 | 陈国忠 | Method for preparing concrete high efficiency water reducing agent by using paper pulp thin black liquor to modify and graft carbonyl aliphatic compound |
| CN102320768A (en) * | 2011-06-20 | 2012-01-18 | 河北久强建材有限公司 | Method for preparing modified aliphatic water reducing agent |
| CN102690076A (en) * | 2011-03-25 | 2012-09-26 | 杨更亮 | Novel high efficiency water reducing agents and preparation technology thereof |
| US20130096285A1 (en) * | 2009-06-19 | 2013-04-18 | Xueqing Qiu | Highly efficient lignin-based water-reducing agent with high degree of sulfonation and high molecular weight, and preparation method thereof |
| CN103359967A (en) * | 2013-07-18 | 2013-10-23 | 安徽森普新型材料发展有限公司 | Aliphatic superplasticizer and preparation method thereof |
| CN105819728A (en) * | 2016-03-10 | 2016-08-03 | 安徽鑫固环保股份有限公司 | Papermaking black liquor modified sulfamate high efficiency water reducer and preparation method thereof |
-
2018
- 2018-05-18 CN CN201810482486.5A patent/CN108609886A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234865A (en) * | 2007-08-22 | 2008-08-06 | 陈国忠 | Method for preparing concrete high efficiency water reducing agent by using paper pulp thin black liquor to modify and graft carbonyl aliphatic compound |
| US20130096285A1 (en) * | 2009-06-19 | 2013-04-18 | Xueqing Qiu | Highly efficient lignin-based water-reducing agent with high degree of sulfonation and high molecular weight, and preparation method thereof |
| CN102690076A (en) * | 2011-03-25 | 2012-09-26 | 杨更亮 | Novel high efficiency water reducing agents and preparation technology thereof |
| CN102320768A (en) * | 2011-06-20 | 2012-01-18 | 河北久强建材有限公司 | Method for preparing modified aliphatic water reducing agent |
| CN103359967A (en) * | 2013-07-18 | 2013-10-23 | 安徽森普新型材料发展有限公司 | Aliphatic superplasticizer and preparation method thereof |
| CN105819728A (en) * | 2016-03-10 | 2016-08-03 | 安徽鑫固环保股份有限公司 | Papermaking black liquor modified sulfamate high efficiency water reducer and preparation method thereof |
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