Straw raw material pretreatment and sulfonation-hydroxymethylation modification method for straw-based water reducing agent

A technology of hydroxymethylation and pretreatment, which is applied in the field of straw raw material pretreatment and sulfonation-hydroxymethylation modification of straw-based water reducing agent, can solve the problem that the degree and method of straw pulverization are not proposed for fine crushing, and no industrialization is proposed. Test ideas and concepts, insufficient utilization of straw raw materials, etc., to achieve the effects of easy industrial application, low cost, and increased reactive area

Active Publication Date: 2020-08-28
TIANSHUI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The water-reducing agent prepared by this method has a low water-reducing rate and can only be used as the most common water-reducing agent
Chinese Patent CN 101759856 B "Preparation Method of Sodium Lignosulfonate Water Reducer", using corn cob, corn cob acid hydrolysis residue, bagasse or corn stalks as raw materials to produce black liquor after alkali boiling, after coarse filtration and ultrafiltration Membrane concentration, sulfonation and spray drying to prepare sodium lignosulfonate superplasticizer with low water content. This process has no pollution to the environment, simple process and low cost, but the raw material of straw cannot be fully utilized and the waste is serious
However, the results of these two studies are just laboratory shake-flask experiments. One is that the degree and method of crushing the straw are not proposed, only the straw is crushed. Bringing in excess chloride ions and sulfate ions will affect the performance of the water reducer. Third, there is no idea and idea for industrial testing, and there is still a long way to go from industrial production equipment and production systems.

Method used

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  • Straw raw material pretreatment and sulfonation-hydroxymethylation modification method for straw-based water reducing agent
  • Straw raw material pretreatment and sulfonation-hydroxymethylation modification method for straw-based water reducing agent
  • Straw raw material pretreatment and sulfonation-hydroxymethylation modification method for straw-based water reducing agent

Examples

Experimental program
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Effect test

Embodiment 1

[0018] A method for pretreatment of straw raw materials and sulfonation-methylolation modification of straw-based water reducer, the specific steps are as follows:

[0019] 1. Primary crushing After a certain amount of raw material straw bales are air-dried naturally, they are crushed into 1-3cm straw segments;

[0020] 2. Cleaning: Clean the silt and other impurities in the straw section after primary crushing;

[0021] 3. Drying The cleaned straw section is dried to keep the moisture content below 10%;

[0022] 4. Secondary crushing: crush the dried straw section into 1-10mm straw section;

[0023] 5. Fine crushing The straw section after secondary crushing is finely crushed by a ball mill, so that the output particle size of the crushed raw material is below 400 μm. The ball mill is a horizontal ball mill, and the particle size of the straw raw material is below 10mm, and the speed is 10-50r / min. 15Kg, 1500 balls, including 1000 copper balls with a diameter of 10mm, 500 c...

Embodiment 2

[0030] A method for pretreatment of straw raw materials and sulfonation-methylolation modification of straw-based water reducer, the specific steps are as follows:

[0031] Steps one, two, three, four, and five are the same as in Example 1, and will not be repeated; the lubricating additive described in step six is ​​stearic acid, and the solid agent ratio of straw and stearic acid is 1000g: 10mL; The main catalytic acid for hydrolysis is itaconic acid, and the ratio of straw to itaconic acid is 1000g: (45-55) mL, more preferably 1000 g: 50 mL; Hydrochloric acid, the proportioning of straw and dilute hydrochloric acid is 1000g: 100mL; All the other are the same as embodiment 1, no longer repeat; The proportioning of solution is 1000g: (30-45) mL, further preferred straw and potassium permanganate solution are 1000g: 40mL; All the other are the same as Example 1, no longer repeat; The sulfonating agent described in step 8 is mass Concentration 50% sodium sulfite, the proportio...

Embodiment 3

[0033] A method for pretreatment of straw raw materials and sulfonation-methylolation modification of straw-based water reducer, the specific steps are as follows:

[0034] Steps 1, 2, 3, 4 and 5 are the same as in Example 1, and will not be repeated; the lubricating additive described in step 6 is a mixture of stearic acid and oleic acid each accounting for 50%, and the solid agent ratio of straw and lubricating additive 1000 g: 8mL; the main catalytic acid for hydrolysis is citric acid, and the ratio of straw and citric acid is 1000g: (30-35) mL, further 1000g: 35mL; the mass concentration of the catalytic promoter for hydrolysis is 30g / L dilute sulfuric acid and dilute hydrochloric acid respectively account for 50% mixed acid, the proportioning of stalks and procatalyst acid is 1000g: 100mL; All the other are the same as embodiment 1, no longer repeat; The oxidizing agent described in the step 7 is mole Potassium permanganate with a concentration of 1.0M and hydrogen peroxi...

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Abstract

The invention discloses a straw raw material pretreatment and sulfonation-hydroxymethylation modification method for a straw-based water reducing agent. A precursor straw lignocellulose pretreatment and sulfonation-hydroxymethylation modification material meeting the requirements of the straw-based water reducing agent is prepared. The method comprises the following steps: 1) primary crushing: crushing into straw sections of about 1-3cm; 2) cleaning: cleaning impurities such as mud and sand; 3) drying: drying to enable the moisture content to be below 10%; 4) secondary crushing: crushing the straw into straw sections of 1-10 mm; 5) micro-crushing: enabling the discharging granularity to be below 400 microns through a ball mill; 6) hydrolyzing: adding a lubricating additive, a main catalytic acid and a co-catalytic acid into the extruder for hydrolysis, 7) oxidizing: adding an oxidant into the extruder for an oxidation chain-breaking reaction, 8) sulfonating: adding a sulfonating agentinto the extruder for a reaction, 9) alkalizing: adding an alkali liquor into the extruder for a reaction, and 10) hydroxymethylating: adding a hydroxymethylation reagent into the extruder for a reaction.

Description

technical field [0001] The invention relates to the technical field of straw raw material pretreatment and sulfonation modification of crop straw-based biomass water reducer precursors, in particular to a straw-based water reducer straw raw material pretreatment and sulfonation-hydroxymethylation modification method. Background technique [0002] At present, with the increasing shortage of petrochemical raw materials required for the preparation of a new generation of high-performance petroleum-based polycarboxylate superplasticizers for concrete admixtures, the price has been rising all the way and the gradual depletion of high-quality concrete aggregates has forced the use of mud content. The prominent problem of high-quality and low-quality sand and gravel aggregates restricts the rapid development of a new generation of high-performance polycarboxylate superplasticizers, making its production costs continue to rise and the high content of sand and gravel in concrete. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C04B20/02C08H8/00D21B1/02D01C1/00
CPCC04B20/023C08H8/00D01C1/00D21B1/02C04B18/248C04B20/026
Inventor 章德玉张惠琴张建斌朱元成唐慧安王鹏刘岿司长代王小芳刘新文雷新有吕玲玲李志锋郭峰左国防杨玲娟刘流
Owner TIANSHUI NORMAL UNIV
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