CN108623769A - The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer - Google Patents
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer Download PDFInfo
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- CN108623769A CN108623769A CN201810482444.1A CN201810482444A CN108623769A CN 108623769 A CN108623769 A CN 108623769A CN 201810482444 A CN201810482444 A CN 201810482444A CN 108623769 A CN108623769 A CN 108623769A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G16/00—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00
- C08G16/02—Condensation polymers of aldehydes or ketones with monomers not provided for in the groups C08G4/00 - C08G14/00 of aldehydes
- C08G16/04—Chemically modified polycondensates
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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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
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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
- 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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Abstract
The present invention relates to prepare modified naphthalene superplasticizer technical field, and in particular to the method that the heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, its step are as follows：First crude naphthalene is added in four-hole boiling flask, is heated to melting, after having melted completely, the industrial concentrated sulfuric acid is added dropwise while stirring, drop is kept the temperature after finishing and detects its acidity value；Cool down certain temperature again, adds suitable water according to acidity value, rectifying heavy distillat is added after the completion of hydrolysis and stirs；Start that formalin is added dropwise after stirring, a period of time is kept the temperature after being added dropwise, liquid caustic soda is slowly added to after heat preservation and adjusts pH value；It is more complex that the present invention solves the heavy distillat recovery processing generated in ethyl alcohol distillation process, it is not disposable, energy consumption is big, the problems such as of high cost, the present invention is in the condensation process grafted naphthalene series high-efficiency water-reducing agent, increase branch quantity, the type in naphthalene series high-efficiency water-reducing agent, so as to improve the water-reducing rate of concrete and improve slump effect.
Description
Technical field
The present invention relates to prepare modified naphthalene superplasticizer technical field, and in particular to the double distilled in ethanol production process
Divide the method for preparing modified naphthalene superplasticizer.
Background technology
China is grain big country, and Ethanol Production by Fermentation has just occurred in China from way back.Currently used work
The method of industry production ethyl alcohol has fermentation method and ethylene synthase method.Either which kind of method ethyl alcohol is both needed to the process pair by rectifying
Ethyl alcohol is purified, and the heavy distillat generated in distillation process is not generally directly discharged to the external world by processing, to environment
Pollution and damage certain caused by equal with human body, while complex to heavy distillat recovery processing step in the prior art, place
Reason difficulty is big, and big energy-consuming is of high cost etc.；Containing ingredients such as ether, ketone, aldehyde, alcohol, lignin in heavy distillat, also have in the prior art
Naphthalene series high-efficiency water-reducing agent is not modified using heavy distillat.
Invention content
(1) the technical issues of solving
In view of the deficiencies of the prior art, it is more multiple to solve the heavy distillat recovery processing generated in ethyl alcohol distillation process by the present invention
Miscellaneous, not disposable, energy consumption is big, it is of high cost the problems such as, while present invention introduces rectifying heavy distillat in ether, ketone, aldehyde, alcohol, wooden
Elements etc. can participate in polymerizeing containing ehter bond, carbonyl, hydroxyl etc., can be grafted to naphthalene series high-efficiency water-reducing agent in condensation course,
Increase branch quantity, the type in naphthalene series high-efficiency water-reducing agent, so as to improve the water-reducing rate of concrete and improve collapsing for concrete
Degree of falling effect.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, includes the following steps：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 155-160
The industrial concentrated sulfuric acid is added dropwise at a temperature of DEG C while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 100-115 DEG C of temperature after stirring, control rate of addition 1.5-3h is added
Finish, a period of time is kept the temperature after being added dropwise, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 7-9 can be prepared by modified naphthalene series
High efficiency water reducing agent.
Preferential, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：200-350 parts of crude naphthalene,
Industrial concentrated sulfuric acid 220-400 parts, 50-100 parts of rectifying heavy distillat, 150-200 parts of formalin, 400-600 parts of liquid caustic soda and water
5-50 parts.
Preferential, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：250-300 parts of crude naphthalene,
Industrial concentrated sulfuric acid 250-350 parts, 60-90 parts of rectifying heavy distillat, 160-180 parts of formalin, 450-550 parts of liquid caustic soda and water
10-40 parts.
Preferential, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：280 parts of crude naphthalene, industry
30 parts of 310 parts of the concentrated sulfuric acid, 80 parts of rectifying heavy distillat, 170 parts of formalin, 500 parts of liquid caustic soda and water.
Preferential, mass fraction is not less than 92.5% shared by the sulfuric acid in the industry concentrated sulfuric acid, the formalin
Mass fraction be 37%.
Preferential, 3-5h is kept the temperature at a temperature of 155-160 DEG C after the dropwise addition industry concentrated sulfuric acid in the step a.
Preferential, 2-5h is kept the temperature at a temperature of 100-115 DEG C after formalin is added dropwise in the step c.
(3) advantageous effect
1, the present invention is directly using the heavy distillat generated in ethyl alcohol distillation process, without being directly used in conjunction through any processing
Pollution of the waste discharge to environment is avoided at modified aliphatic high efficiency water reducing agent, and it is more multiple to solve heavy distillat recovery processing
Miscellaneous, not disposable, energy consumption is big, it is of high cost the problems such as, belong to the environment-friendly type invention of hazardous waste recycling.
2, present invention introduces rectifying heavy distillat in ether, ketone, aldehyde, alcohol, lignin etc. containing ehter bond, carbonyl, hydroxyl etc. is equal
It can participate in polymerizeing, naphthalene series high-efficiency water-reducing agent can be grafted in condensation course, increase the branch in naphthalene series high-efficiency water-reducing agent
Quantity, type, so as to improve the water-reducing rate of concrete and improve the slump effect of concrete.
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：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 155 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 100 DEG C of temperature after stirring, control rate of addition 1.5h adds complete, dropwise addition
After keep the temperature a period of time, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 7.5 can be prepared by modified naphthalene series and efficiently subtract
Aqua.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：200 parts of crude naphthalene, industrial 220 parts of the concentrated sulfuric acid,
20 parts of 70 parts of rectifying heavy distillat, 150 parts of formalin, 400 parts of liquid caustic soda and water.
Embodiment 2：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 160 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 115 DEG C of temperature after stirring, control rate of addition 2h adds complete, dropwise addition
After keep the temperature a period of time, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 8 can be prepared by the efficient diminishing of modified naphthalene series
Agent.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：250 parts of crude naphthalene, industrial 260 parts of the concentrated sulfuric acid,
35 parts of 70 parts of rectifying heavy distillat, 180 parts of formalin, 500 parts of liquid caustic soda and water.
Embodiment 3：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 155 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 115 DEG C of temperature after stirring, control rate of addition 3h adds complete, dropwise addition
After keep the temperature a period of time, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 9 can be prepared by the efficient diminishing of modified naphthalene series
Agent.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：310 parts of crude naphthalene, industrial 300 parts of the concentrated sulfuric acid,
40 parts of 80 parts of rectifying heavy distillat, 190 parts of formalin, 550 parts of liquid caustic soda and water.
Embodiment 4：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 160 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 100 DEG C of temperature after stirring, control rate of addition 2h adds complete, dropwise addition
After keep the temperature a period of time, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 8 can be prepared by the efficient diminishing of modified naphthalene series
Agent.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：320 parts of crude naphthalene, industrial 370 parts of the concentrated sulfuric acid,
45 parts of 80 parts of rectifying heavy distillat, 170 parts of formalin, 530 parts of liquid caustic soda and water.
Embodiment 5：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 155 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 115 DEG C of temperature after stirring, control rate of addition 2.5h adds complete, drop
A period of time is kept the temperature after adding, and liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 9 can be prepared by modified naphthalene series and efficiently subtract
Aqua.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：310 parts of crude naphthalene, industrial 340 parts of the concentrated sulfuric acid,
30 parts of 100 parts of rectifying heavy distillat, 200 parts of formalin, 550 parts of liquid caustic soda and water.
Embodiment 6：
The method that heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, steps are as follows：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 160 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, has hydrolyzed
At rear addition rectifying heavy distillat, 30min is stirred；
C, start that formalin is added dropwise in 115 DEG C of temperature after stirring, control rate of addition 3h adds complete, dropwise addition
After keep the temperature a period of time, liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that 9 can be prepared by the efficient diminishing of modified naphthalene series
Agent.
Modified naphthalene superplasticizer is made by the raw material of following parts by weight：280 parts of crude naphthalene, industrial 310 parts of the concentrated sulfuric acid,
30 parts of 80 parts of rectifying heavy distillat, 170 parts of formalin, 500 parts of liquid caustic soda and water.
The present invention selects common naphthalene water reducer to be added in concrete mix as an aqueous solution, and (its volume is water
The 1.6% of mud weight) as control group, product made from embodiment 1-6 is added in concrete mix as an aqueous solution
(its volume is the 1.6% of cement weight) it is as shown in table 1 to obtain properties data under the same conditions as experimental group：
Table 1
As shown in Table 1, the product of the 1-6 of the embodiment of the present invention is being added to concrete mix as an aqueous solution
Shi Junneng improves the water-reducing rate of concrete and improves the slump effect of concrete, and the product water-reducing rate highest of the present embodiment 6 is simultaneously
And the slump effect for improving concrete is the most apparent.
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 by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including 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 (7)
1. the method that the heavy distillat in ethanol production process prepares modified naphthalene superplasticizer, which is characterized in that including following
Step：
A, first crude naphthalene is added in four-hole boiling flask, 150 DEG C of meltings is heated to, after having melted completely, in 155-160 DEG C of temperature
The industrial concentrated sulfuric acid is added dropwise under degree while stirring, 30min is dripped off, and drop is kept the temperature after finishing and detects its acidity value；
B, the product in step a is cooled to 120 DEG C, suitable water is added according to acidity value, 30min is hydrolyzed, after the completion of hydrolysis
Rectifying heavy distillat is added, stirs 30min；
C, start that formalin is added dropwise in 100-115 DEG C of temperature after stirring, control rate of addition 1.5-3h adds complete, drop
A period of time is kept the temperature after adding, and liquid caustic soda is slowly added to after heat preservation and adjusts pH value to be that can be prepared by modified naphthalene series efficient by 7-9
Water-reducing agent.
2. the method that the heavy distillat in ethanol production process as described in claim 1 prepares modified naphthalene superplasticizer,
It is characterized in that, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：200-350 parts of crude naphthalene, industry are dense
5-50 parts of 220-400 parts of sulfuric acid, 50-100 parts of rectifying heavy distillat, 150-200 parts of formalin, 400-600 parts of liquid caustic soda and water.
3. the method that the heavy distillat in ethanol production process as claimed in claim 2 prepares modified naphthalene superplasticizer,
It is characterized in that, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：250-300 parts of crude naphthalene, industry are dense
10-40 parts of 250-350 parts of sulfuric acid, 60-90 parts of rectifying heavy distillat, 160-180 parts of formalin, 450-550 parts of liquid caustic soda and water.
4. the method that the heavy distillat in ethanol production process as claimed in claim 2 prepares modified naphthalene superplasticizer,
It is characterized in that, the modified naphthalene superplasticizer is made by the raw material of following parts by weight：280 parts of crude naphthalene, the industrial concentrated sulfuric acid
30 parts of 310 parts, 80 parts of rectifying heavy distillat, 170 parts of formalin, 500 parts of liquid caustic soda and water.
5. the method that the heavy distillat in ethanol production process as described in claim 1 prepares modified naphthalene superplasticizer,
It is characterized in that：Mass fraction is not less than 92.5% shared by sulfuric acid in the industry concentrated sulfuric acid, the quality of the formalin
Score is 37%.
6. the method that the heavy distillat in ethanol production process as described in claim 1 prepares modified naphthalene superplasticizer,
It is characterized in that：3-5h is kept the temperature at a temperature of 155-160 DEG C after the dropwise addition industry concentrated sulfuric acid in the step a.
7. the method that the heavy distillat in ethanol production process as described in claim 1 prepares modified naphthalene superplasticizer,
It is characterized in that：2-5h is kept the temperature at a temperature of 100-115 DEG C after formalin is added dropwise in the step c.
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Cited By (1)
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| CN108586683A (en) * | 2018-05-18 | 2018-09-28 | 萧县沃德化工科技有限公司 | The method that heavy distillat prepares modified aliphatic high efficiency water reducing agent in ethanol production process |
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| US20060134335A1 (en) * | 2004-12-17 | 2006-06-22 | David Glassel | Methods for preventing warping in wood products |
| CN101054272A (en) * | 2007-04-11 | 2007-10-17 | 中建三局建设工程股份有限公司商品混凝土公司 | Method for producing herbage black liquor modified high efficiency water reducing agent |
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Application publication date: 20181009 |