CN103121807B - Preparation method of concrete slump retaining agent - Google Patents
Preparation method of concrete slump retaining agent Download PDFInfo
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- CN103121807B CN103121807B CN201110366614.8A CN201110366614A CN103121807B CN 103121807 B CN103121807 B CN 103121807B CN 201110366614 A CN201110366614 A CN 201110366614A CN 103121807 B CN103121807 B CN 103121807B
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Abstract
The invention belongs to the field of cement additives and particularly relates to a preparation method of concrete slump retaining agent. The method includes the steps of firstly, adding straw hydrolyzed sugar into chemical oxidant, and feeding air for reaction; secondly, at normal temperature, adding chemical oxidant C, dropwise adding lye to allow system Ph to be 7-8, and allowing for reaction; thirdly, adding noble metal catalyst, and dropwise adding lye to allow system Ph to be 8-8.5 to obtain the concrete slump retaining agent; wherein the chemical oxidant includes chemical oxidant A and chemical oxidant B; the weight ratio of the straw hydrolyzed sugar, the chemical oxidant A and the chemical oxidant B is 800-1200:2-30:1-8; reaction temperature is 30-80 DEG C; and reaction time is 1-3 hours. The preparation method is good in product quality, low in cost, low in catalyst consumption, and stable in reaction.
Description
Technical field
The invention belongs to cement additire field, particularly relate to a kind of preparation method of concrete slump retaining agent.
Background technology
Slump retaining agent is the admixture that can keep concrete slump not immediate loss.Slump retaining agent is in fact retardant, delays hydrated cementitious condensation, reaches the effect keeping the slump.Ordinary water-reducing agent wood calcium or wooden sodium and polycarboxylic acid series special superplasticizer, itself has delayed coagulation, generally protects the effectiveness comparison that collapses good.For naphthalene series high-efficiency water-reducing agent, often need composite guarantor to collapse composition, or need on-the-spot secondary to add, otherwise slump-loss is fast, constructional difficulties.If envrionment temperature is high, and concrete haul distance is long, then should use slump retaining agent or retardant, can reach very good effect.
Adopt the oxidation of stalk hydrolysis sugar to prepare concrete slump retaining agent and there is practice significance.At present, the method for the carboxylate salt of glycoxidative sugaring has: biological fermentation process, electrolytic oxidation, chemical oxidizing agent homogeneous oxidizing method, precious metal catalyst heterogeneous oxidation method.In industrialized production method, more than 80% is adopt precious metal catalyst heterogeneous oxidation method, although this method technique is simple, and reacting balance, be easy to control, reaction conditions is gentle, transformation efficiency high (98%); But Problems existing is also very large, show that catalyst recirculation uses catalytic rate after certain number of times to decline, easy poisoning and deactivation in catalyzer use procedure and substantially increase production cost, the consumption of general catalyzer is 1 ~ 2% of saccharic amount, how to reduce the most important research direction that catalyst levels has just become this field.
Summary of the invention
The present invention is intended to overcome the deficiencies in the prior art part and provide a kind of object product qualities good, and with low cost, catalyst levels is little, the preparation method of the concrete slump retaining agent of reacting balance.
For solving the problems of the technologies described above, the present invention realizes like this.
The preparation method of concrete slump retaining agent, can implement as follows.
(1) stalk hydrolysis sugar is added chemical oxidizing agent, and pass into air and react.
(2) under constant temperature, add chemical oxidizing agent C, drip alkali lye simultaneously and make system Ph=7 ~ 8, react.
(3) add noble metal catalyst, drip alkali lye and make system Ph=8 ~ 8.5, spraying dry, obtain object product.
As a kind of preferred version, in step of the present invention (1), chemical oxidizing agent is chemical oxidizing agent A and chemical oxidizing agent B; The weight ratio of described stalk hydrolysis sugar, chemical oxidizing agent A and chemical oxidizing agent B is: 800 ~ 1200:2 ~ 30:1 ~ 8.
As another kind of preferred version, in step of the present invention (1), temperature of reaction is: 30 ~ 80 DEG C; Reaction times is: 1 ~ 3 hour.
Further, in step of the present invention (1), air pressure is: 0.11 ~ 0.14MPa.
Further, in step of the present invention (2), the reaction times is: 1 ~ 3 hour; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C is: 800 ~ 1200:2 ~ 30:1 ~ 8:2 ~ 20; Air pressure is: 0.11 ~ 0.14MPa.
In addition, in step of the present invention (3), air pressure is: 0.13 ~ 0.18MPa; Temperature of reaction is: 40 ~ 60 DEG C; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B, chemical oxidizing agent C and noble metal catalyst is: 800 ~ 1200:2 ~ 30:1 ~ 8:2 ~ 20:0.3 ~ 2.
Secondly, chemical oxidizing agent A of the present invention, chemical oxidizing agent B and chemical oxidizing agent C adopt hydrogen peroxide, Hydrogen bromide, ammonium persulphate, potassium permanganate, clorox, SPC-D or Sodium peroxoborate.
Again, noble metal catalyst of the present invention is: one or more the mixture in palladium-carbon catalyst, ruthenium C catalyst or palladium bismuth C catalyst.
The object of the invention product qualities is good, with low cost, and catalyst levels is little, reacting balance.The air oxidation process that first paragraph system of the present invention is catalyzer with ternary chemical oxidizing agent; Second segment adds a small amount of remaining sugar of noble metal catalyst atmospheric oxidation again, and the transformation efficiency that final glycosyloxy turns to carboxylic acid can reach 95% ~ 98%.Detect by analysis and learn, the effect of the concrete slump retaining agent that this transformation efficiency obtains is completely up to standard, the diversified development trend of concrete to retardant performance requirement can be adapted to better, this is relevant containing a part five yuan of sugar with retardant, has certain regularity between the oxidation ratio of sugar and the performance of retardant.The best oxygen rate scope of stalk sugar is 70% ~ 95%.Which achieves the object reducing noble metal catalyst consumption.Experiment shows, noble metal catalyst consumption is only 1/10th of traditional technology.
Embodiment
Embodiment 1.
The preparation method of concrete slump retaining agent, can implement as follows.
(1) stalk hydrolysis sugar is added chemical oxidizing agent, and pass into air and react.
(2) under constant temperature, add chemical oxidizing agent C, drip alkali lye simultaneously and make system Ph=8, react.
(3) add noble metal catalyst, drip alkali lye and make system Ph=8.5, spraying dry, obtain object product.
In above-mentioned steps (1), chemical oxidizing agent is chemical oxidizing agent A and chemical oxidizing agent B; The weight ratio of described stalk hydrolysis sugar, chemical oxidizing agent A and chemical oxidizing agent B is: 1000:15:7, and temperature of reaction is: 70 DEG C; Reaction times is: 2 hours, and air pressure is: 0.13MPa.
In above-mentioned steps (2), the reaction times is: 2 hours; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C is: 1000:15:7:13; Air pressure is: 0.13MPa.
In above-mentioned steps (3), air pressure is: 0.15MPa; Temperature of reaction is: 50 DEG C; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B, chemical oxidizing agent C and noble metal catalyst is: 1000:15:7:13:1.
Above-mentioned chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C adopt hydrogen peroxide, Hydrogen bromide or ammonium persulphate.
Above-mentioned noble metal catalyst is: palladium-carbon catalyst.
Embodiment 2.
The preparation method of concrete slump retaining agent, can implement as follows.
(1) stalk hydrolysis sugar is added chemical oxidizing agent, and pass into air and react.
(2) under constant temperature, add chemical oxidizing agent C, drip alkali lye simultaneously and make system Ph=7, react.
(3) add noble metal catalyst, drip alkali lye and make system Ph=8, spraying dry, obtain object product.
In above-mentioned steps (1), chemical oxidizing agent is chemical oxidizing agent A and chemical oxidizing agent B; The weight ratio of described stalk hydrolysis sugar, chemical oxidizing agent A and chemical oxidizing agent B is: 800:14:5.
In above-mentioned steps (1), temperature of reaction is: 35 DEG C; Reaction times is: 2 hours, and air pressure is: 0.12MPa.
In above-mentioned steps (2), the reaction times is: 1.5 hours; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C is: 800:14:5:15; Air pressure is: 0.14MPa.
In above-mentioned steps (3), air pressure is: 0.16MPa; Temperature of reaction is: 55 DEG C; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B, chemical oxidizing agent C and noble metal catalyst is: 800:14:5:15:0.5.
Above-mentioned chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C adopt clorox, SPC-D or Sodium peroxoborate.
Above-mentioned noble metal catalyst is: ruthenium C catalyst.
Embodiment 3.
The preparation method of concrete slump retaining agent, is characterized in that, implements as follows.
(1) stalk hydrolysis sugar is added chemical oxidizing agent, and pass into air and react.
(2) under constant temperature, add chemical oxidizing agent C, drip alkali lye simultaneously and make system Ph=7.5, react.
(3) add noble metal catalyst, drip alkali lye and make system Ph=8.1, spraying dry, obtain object product.
In above-mentioned steps (1), chemical oxidizing agent is chemical oxidizing agent A and chemical oxidizing agent B; The weight ratio of described stalk hydrolysis sugar, chemical oxidizing agent A and chemical oxidizing agent B is: 860:11:6.
In above-mentioned steps (1), temperature of reaction is: 60 DEG C; Reaction times is: 2 hours, and air pressure is: 0.11MPa.
In above-mentioned steps (2), the reaction times is: 2 hours; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C is: 860:11:6:11; Air pressure is: 0.13MPa.
In above-mentioned steps (3), air pressure is: 0.15MPa; Temperature of reaction is: 45 DEG C; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B, chemical oxidizing agent C and noble metal catalyst is: 860:11:6:11:0.8.
Above-mentioned chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C adopt ammonium persulphate.
Above-mentioned noble metal catalyst is: palladium bismuth C catalyst.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (1)
1. the preparation method of concrete slump retaining agent, is characterized in that, implements as follows:
Stalk hydrolysis sugar is added chemical oxidizing agent, and passes into air and react; Chemical oxidizing agent is chemical oxidizing agent A and chemical oxidizing agent B; The weight ratio of described stalk hydrolysis sugar, chemical oxidizing agent A and chemical oxidizing agent B is: 800 ~ 1200:2 ~ 30:1 ~ 8; Temperature of reaction is: 30 ~ 80 DEG C; Reaction times is: 1 ~ 3 hour; Air pressure is: 0.11 ~ 0.14MPa;
(2) under constant temperature, add chemical oxidizing agent C, drip alkali lye simultaneously and make system pH=7 ~ 8, react; Reaction times is: 1 ~ 3 hour; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C is: 800 ~ 1200:2 ~ 30:1 ~ 8:2 ~ 20; Air pressure is: 0.11 ~ 0.14MPa;
(3) add noble metal catalyst, drip alkali lye and make system pH=8 ~ 8.5, spraying dry, obtain object product; Air pressure is: 0.13 ~ 0.18MPa; Temperature of reaction is: 40 ~ 60 DEG C; The weight ratio of stalk hydrolysis sugar, chemical oxidizing agent A, chemical oxidizing agent B, chemical oxidizing agent C and noble metal catalyst is: 800 ~ 1200:2 ~ 30:1 ~ 8:2 ~ 20:0.3 ~ 2;
Described chemical oxidizing agent A, chemical oxidizing agent B and chemical oxidizing agent C adopt hydrogen peroxide, Hydrogen bromide, ammonium persulphate, potassium permanganate, clorox, SPC-D or Sodium peroxoborate; Described noble metal catalyst is: one or more the mixture in palladium-carbon catalyst, ruthenium C catalyst or palladium bismuth C catalyst.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201110366614.8A CN103121807B (en) | 2011-11-18 | 2011-11-18 | Preparation method of concrete slump retaining agent |
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| CN201110366614.8A CN103121807B (en) | 2011-11-18 | 2011-11-18 | Preparation method of concrete slump retaining agent |
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| CN103121807A CN103121807A (en) | 2013-05-29 |
| CN103121807B true CN103121807B (en) | 2015-03-04 |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102229478A (en) * | 2011-04-08 | 2011-11-02 | 江苏博特新材料有限公司 | Preparation method of molasses retarding water reducer and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102229478A (en) * | 2011-04-08 | 2011-11-02 | 江苏博特新材料有限公司 | Preparation method of molasses retarding water reducer and application thereof |
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