阅读说明：本技术 磺化-羟甲基化改性的秸秆基减水剂的制备方法和装置 (Preparation method and device of sulfonated-hydroxymethylated modified straw-based water reducing agent ) 是由 章德玉 张惠琴 刘流 王鹏 刘岿 司长代 张建斌 唐慧安 左国防 王小芳 刘新文 于 2019-02-21 设计创作，主要内容包括：本发明为磺化-羟甲基化改性的秸秆基减水剂的制备方法和装置。是通过改性制备秸秆基生物质减水剂的方法和设备。旨在通过对秸秆原料的预处理和磺化-羟甲基化改性,制备出生物质减水剂。其制备方法由秸秆原料预处理和磺化-羟甲基化改性两部分组成,秸秆预处理包括初碎、清洗、干燥、二次粉碎、微碎和水解过程；磺化-羟甲基化改性由物料氧化断链、磺化改性、碱化和羟甲基化改性组成。所用设备包括初碎、清洗、干燥装置、旋风分离器、二次粉碎、微碎装置、集料仓称重装置、螺旋挤出水解机、配料储罐、螺旋挤出改性反应机组和储料罐。本发明用于制备秸秆基生物质减水剂。(The invention relates to a preparation method and a device of a sulfonated-hydroxymethylated modified straw-based water reducing agent. Is a method and equipment for preparing a straw-based biomass water reducing agent by modification. Aims to prepare the biomass water reducing agent by pretreatment and sulfonation-hydroxymethylation modification of straw raw materials. The preparation method comprises two parts of pretreatment of straw raw materials and sulfonation-hydroxymethylation modification, wherein the pretreatment of the straw comprises the processes of primary crushing, cleaning, drying, secondary crushing, micro crushing and hydrolysis; the sulfonation-hydroxymethylation modification is composed of material oxidation chain scission, sulfonation modification, alkalization and hydroxymethylation modification. The equipment comprises a primary crushing device, a cleaning device, a drying device, a cyclone separator, a secondary crushing device, a micro-crushing device, a material collecting bin weighing device, a spiral extrusion hydrolysis machine, a batching storage tank, a spiral extrusion modification reaction unit and a storage tank. The method is used for preparing the straw-based biomass water reducing agent.)

1. The preparation method of the sulfonation-hydroxymethylation modified straw-based water reducing agent is characterized by comprising two parts of straw raw material pretreatment and sulfonation-hydroxymethylation modification, wherein the straw raw material pretreatment comprises the steps of straw raw material primary crushing, cleaning, drying, secondary crushing, micro crushing and hydrolysis, and the sulfonation-hydroxymethylation modification method comprises the following steps of material oxidation chain scission, sulfonation modification, alkalization and hydroxymethylation modification:

1) pretreatment of straw raw materials:

1.1, naturally drying a certain amount of raw material straw bundles, and crushing the raw material straw bundles into 1-3 cm straw sections by a primary crushing device;

1.2 cleaning the primarily crushed straw sections by a cleaning device to remove impurities such as quicksand and the like;

1.3, further drying by a drying device consisting of a pre-drying device and a spiral dryer to ensure that the water content of the straws is below 10 percent by mass;

1.4, crushing the dried straw sections into straw sections of 1-10 mm by a secondary crushing device;

1.5, performing ball milling and fine crushing on the straw sections subjected to secondary crushing by a horizontal ball mill micro-crushing device, and stopping ball milling when the discharge granularity is below 400 mu m;

1.6, hydrolysis treatment of straw powder:

1.6.1 weighing a certain amount of the straw powder obtained in the section 1.5 through a No. 1 aggregate bin, and feeding the straw powder into a screw extrusion hydrolysis machine for hydrolysis;

1.6.2 in the hydrolysis process, firstly, a heater is started to heat the machine body by hot water through a coil heat exchanger, and then ingredients are added;

1.6.3 materials enter a spiral extrusion hydrolysis machine, then the flow is controlled to slowly add the 1#, 2# and 3# preparation solutions in the batching storage tank group into the spiral extrusion hydrolysis machine at the same time, and the materials are discharged after thermal insulation and hydrolysis.

2) Straw sulfonation-hydroxymethylation modification method

2.1 weighing a certain amount of straw materials prepared by hydrolysis pretreatment through a 1# aggregate bin weighing device, feeding the weighed straw materials into a reaction unit formed by connecting 1#, 2#, 3# and 4# spiral extruders in series, and carrying out oxidation, sulfonation-hydroxymethylation modification reaction;

2.2 in the modification reaction process, firstly, a heater is started to heat the machine body, so that the materials are heated to about 70 ℃, and then the preparation liquid is sequentially added;

2.3, feeding the material into a No. 1 screw extruder, starting a control valve of a batching storage tank group, slowly adding an oxidant into the No. 1 screw extruder, preserving heat to mix the material, carrying out oxidation chain scission reaction on the straw intrinsic cellulose, and discharging the material into the No. 2 screw extruder after a certain time;

2.4, starting a new round of straw materials to enter a No. 1 screw extruder, and repeating the operation of 2.3 sections to carry out oxidation chain scission reaction;

feeding the 2.51 # spiral extruder into the 2# spiral extruder, adding a sulfonating agent with a certain mass concentration in a 2# batching storage tank, reacting for a certain time, and feeding into the 3# spiral extruder;

2.6 feeding the material into the No. 2 screw extruder by a new round of the No. 1 screw extruder, and repeating the procedure of 2.5 sections to carry out sulfonation modification reaction;

feeding the 2.72 # screw extruder into a 3# screw extruder, adding alkali liquor with a certain concentration dose in a 3# batching storage tank, adjusting the pH value to 8-9, reacting for a certain time, and feeding into a 4# screw extruder;

2.8 feeding the material into a No. 3 screw extruder in a new round of the No. 2 screw extruder, repeating the procedure of 2.7 sections, and adding alkali to adjust the pH value to 8-9;

feeding the 2.93 # screw extruder into a 4# screw extruder, adding a certain mass concentration and a certain dosage of a hydroxymethylation reagent into a 4# batching storage tank, carrying out heat preservation reaction for a certain time, then feeding, weighing by a 2# aggregate bin weighing device, feeding into a storage tank with a trolley, conveying away after reaching a specified weight, and feeding into the next storage tank with the trolley;

2.10 feeding the new 3# screw extruder into the 4# screw extruder, and repeating the procedure of 2.9 to perform hydroxymethylation modification reaction.

2. The preparation method according to claim 1, wherein the No. 1, No. 2 and No. 3 preparation solutions are respectively a lubricant additive, a main catalytic acid and a cocatalyst acid.

3. The method according to claim 1, wherein the sulfonating agent is sodium sulfite at a certain mass concentration.

4. The method according to claim 1, wherein the methylolation reagent is a formaldehyde solution having a certain mass concentration.

5. The utility model provides a preparation facilities of modified straw base water-reducing agent of sulfonation-hydroxymethylation, includes equipment support and storage tank, its characterized in that preparation facilities still includes straw primary crushing device, belt cleaning device, drying device, spiral dryer, cyclone, secondary crushing device, the little comminution device of ball mill, 1# collection feed bin weighing device, spiral extrusion hydrolysis machine, 1# batching storage tank group, 1# heater, 2# collection feed bin weighing device, 2# batching storage tank group, spiral extrusion modification reaction unit, 2# heater, 3# collection feed bin weighing device and the storage tank of taking the shallow, the part is arranged in proper order and is settled, constitutes a complete system.

Technical Field

The invention relates to a method and a device for preparing a straw-based biomass water reducing agent through modification, in particular to a method and a device for preparing a sulfonated-hydroxymethylated modified straw-based water reducing agent.

Background

At present, along with the increasing shortage of petrochemical raw materials required by a new generation of high-performance petroleum-based polycarboxylate water reducer for preparing a concrete admixture, the price is gradually increased and the high-quality aggregate of concrete is gradually consumed, so that the outstanding problem that the use of low-quality sandstone aggregate with high mud content is forced is solved, the rapid development of the new generation of high-performance polycarboxylate water reducer is restricted, the production cost is continuously increased, and the loss of high performance such as high water reduction, high fluidity, high strength, high durability and the like of the polycarboxylate water reducer in concrete is caused by the high mud content of the sandstone in the concrete, the polycarboxylic acid water reducing agent has the defects that the polycarboxylic acid water reducing agent with higher performance advantage than naphthalene water reducing agents, aliphatic water reducing agents, sulfamate water reducing agents, lignin water reducing agents and the like cannot be widely popularized and applied in the building industry to improve the building quality.

With the problems of high cost, low mud resistance and the like of the polycarboxylic acid water reducing agent serving as a novel additive of concrete, the national and foreign scholars begin to research key bottleneck technical problems such as raw material selection, synthesis method and the like of the polycarboxylic acid water reducing agent with low cost, mud resistance and salt resistance in recent years.

The research on the low-cost polycarboxylate water reducer is mainly embodied in that biomass-based renewable raw materials are used as a main method for reducing the polycarboxylate water reducer, the application of modified cellulose, hemicellulose, starch, monosaccharide and the like in the water reducer is mainly reported at present, and the modification methods mainly comprise sulfonation, esterification, etherification, amidation and the like.

Crop straws are inexpensive biomass raw materials which cannot be fully utilized, and comprise the rest parts of wheat, rice, corn, potatoes, oil plants, cotton, sugarcane and other crops after seeds are harvested. China is a big agricultural country, and most of crop straws which are produced by 7 hundred million or more tons per year are still incinerated, so that resource waste and environmental pollution are caused. The utilization of crop straws has been internationally regarded as a strategic industry for developing renewable energy resources in the 21 st century, and the resource utilization of crop straws mainly focuses on the development of chemical engineering and building materials. At present, the application research of crop straws as building materials is a hotspot, for example. However, the research on the direct use of the water reducing agent as a raw material is very rare. The main components of the straw are cellulose, hemicellulose, lignin and other bio-based macromolecules, the molecules contain ether groups, carbon-carbon double bonds, propenol hydroxyl groups, phenolic hydroxyl groups, carbonyl groups, methoxyl groups, carboxyl groups, benzene rings and other functional groups and chemical bonds, graft copolymerization and cross-linking copolymerization reactions such as etherification, esterification, sulfonation, amidation and the like can be carried out, and the obtained product has special performance.

At present, few research reports of directly using biomass straws as a water reducing agent exist, and most of the research reports are that cellulose and lignin are extracted and separated from the straws, or black liquor wastewater obtained by producing paper making and ethanol from the straws is used as a raw material for modification research of the water reducing agent or compounding research with a polycarboxylic acid water reducing agent.

A study on a lignin modified water reducer, CN 101337789A, a method for preparing the water reducer by condensation modification of wheat straw alkali lignin, includes the steps of adding wheat straw alkali lignin into water with the weight of 4.4-5.5 times of that of wheat straw alkali lignin for dissolution, adding copper sulfate with the weight of 0.6-0.9% of that of the wheat straw alkali lignin, adjusting the pH value to 10-11 by using a caustic soda solution, adding anhydrous sodium sulfite with the weight of 45-55% of that of the wheat straw alkali lignin, heating to 88-92 ℃, reacting for 4-5 hours to obtain a sulfonated product, and carrying out condensation reaction on the sulfonated product and quantitative formaldehyde under the conditions of the pH value of 11.6-12.0 and the temperature of 65-75 ℃ to obtain the water reducer. The water reducing agent prepared by the method has low water reducing rate and can only be used as the most common water reducing agent. Chinese patent CN 101759856B "preparation method of sodium lignosulfonate water reducer", takes black liquor produced by soda boiling of corncobs, corncob acid hydrolysis residues, bagasse or corn stalks as raw materials, and prepares the sodium lignosulfonate water reducer with low water content by coarse filtration, ultrafiltration membrane concentration, sulfonation and spray drying. Chinese patent CN 106698993A, "a polycarboxylate water reducing agent", utilizes waste white mud to size, heat, mix with corn stalk again, add sodium dodecyl sulfate, dry and extrude the piece after stirring, the acid leaching obtains the hydrolyzate, utilize CaO to adjust the straw hydrolyzate to pH value 6.0-7.0, the hydrolyzate that obtains is dried, oxidized, sulfonated, add to polycarboxylate water reducing agent, use ultrasonic treatment 1-2 h after stirring evenly, obtain modified polycarboxylate water reducing agent. The method has the main advantages that the papermaking waste liquid is used for preparing the polycarboxylic acid water reducing agent, waste materials can be well changed into valuable materials, and the strong base in the papermaking waste liquid is utilized to pretreat the corn straws, so that the corn straws can be better soaked in acid for hydrolysis. The essence of the method is that lignin in the straws is sulfonated and compounded with a water reducing agent. Chinese patent CN 102936110A, "a lignosulfonate-polycarboxylic acid copolymerization composite high-performance water reducing agent and a preparation method thereof", is obtained by directly synthesizing lignosulfonate, methyl allyl polyoxyethylene ether and acrylic acid under the action of ammonium persulfate and neutralizing with sodium hydroxide. The essence of the water reducing agent is a lignosulfonate modified polycarboxylic acid water reducing agent.

The research of directly using biomass straws as a water reducing agent mainly has two reports at present: chinese patent CN 106279574A 'A polycarboxylate superplasticizer modified by straws and a preparation method thereof', the first step is straw pretreatment: crushing straws, adding dilute acid, uniformly stirring and mixing, soaking for 18-36h, filtering, and washing the straws to be neutral by using clear water; step two, preparing the straw modified polycarboxylate superplasticizer: adding methallyl polyoxyethylene-1000, methallyl polyoxyethylene-2400, maleic anhydride, acrylamide, sodium methallyl sulfonate and straws into a four-reflux device and a constant-pressure dropping funnel, adding ammonium persulfate into the constant-pressure dropping funnel, beginning to drop initiator ammonium persulfate at a dropping speed of 2-4 drops/s, and preserving heat for 4-5 hours after dropping; cooling to 35-45 ℃, and adjusting the pH value to 6.8-7.2 to obtain the straw modified polycarboxylic acid water reducing agent. Chinese patent CN 105713164B, "an aliphatic water-reducing agent prepared from straws and a preparation method thereof", is prepared by the steps of straw acid cleaning, straw modified aliphatic water-reducing agent and the like. The method specifically comprises the following steps: pretreating straws, namely crushing corn straws or wheat straws, adding dilute acid, uniformly stirring and mixing, soaking for 18-36h, filtering, and washing the straws to be neutral by using clear water; adding water into a reaction kettle, then adding sodium sulfite, and dissolving; adding acetone into the dissolved sodium sulfite solution, and sulfonating for 8-12 min; then adding the pretreated straws, and stirring and reacting for 20-40 min; and adding formaldehyde into the solution, and reacting at 90-95 ℃ for 1-2 h to prepare the straw modified aliphatic water reducer. The technology effectively utilizes the straw waste resources, overcomes the defect of poor retarding effect of the existing aliphatic water reducing agent, improves the application range of the aliphatic water reducing agent, and reduces the production cost. However, the two research results are only small-scale shaking tests in laboratories, firstly, the degree and method of fine crushing are not provided for crushing the straws, but the straw crushing is only provided, secondly, excessive chloride ions and sulfate ions are brought in by the hydrolysis of the straws by using conventional dilute hydrochloric acid or dilute sulfuric acid to influence the performance of the water reducing agent, thirdly, the conception and concept of industrial tests are not provided, and a great distance is left between the research results and industrial production devices and production systems.

The water reducing agent is prepared by directly modifying the crop straws, the requirements on the pretreatment method and the modification method of the straw raw materials and corresponding equipment and devices are high, the performance of the subsequently prepared straw-based water reducing agent is directly influenced, the key problem which needs to be considered in the industrial production of the straw water reducing agent is also solved, and otherwise, the development and utilization value of the novel water reducing agent cannot be realized. However, reports on the method for micro-crushing and hydrolysis pretreatment of straw raw materials and a special device for modification such as sulfonation and the like for directly preparing the water reducing agent by using crop straws are not seen yet.

Disclosure of Invention

The invention aims to provide a preparation method and a device of a sulfonated-hydroxymethylated modified straw-based water reducing agent, which are used for preparing a biomass water reducing agent directly used for reducing water by 10-15% by pretreating crop straw raw materials and carrying out sulfonation-hydroxymethylated modification, further promote the industrialization process of a low-cost straw-based biomass concrete water reducing agent, provide new possibility for recycling crop straws, and meet the development strategy of national biomass resources.

The technical scheme of the invention is as follows:

the preparation method of the straw-based water reducing agent comprises two parts, namely straw raw material pretreatment and sulfonation-hydroxymethylation modification, wherein the straw raw material pretreatment comprises the steps of straw raw material primary crushing, cleaning, drying, secondary crushing, micro crushing and hydrolysis, and the sulfonation-hydroxymethylation modification method comprises the steps of material oxidation chain scission, sulfonation modification, alkalization and hydroxymethylation modification;

1. pretreatment of straw raw materials:

1.1, naturally drying a certain amount of raw material straw bundles, and crushing the raw material straw bundles into 1-3 cm straw sections by a primary crushing device;

1.2 cleaning the primarily crushed straw sections by a cleaning device to remove impurities such as quicksand and the like;

1.3, further drying by a drying device consisting of a pre-drying device and a spiral dryer to ensure that the water content of the straws is below 10 percent by mass;

1.4, crushing the dried straw sections into straw sections of 1-10 mm by a secondary crushing device;

1.5, performing ball milling and fine crushing on the straw sections subjected to secondary crushing by a horizontal ball mill micro-crushing device, and stopping ball milling when the discharge granularity is below 400 mu m;

1.6, hydrolysis treatment of straw powder:

1.6.1 weighing a certain amount of the straw powder obtained in the section 1.5 through a No. 1 aggregate bin, and feeding the straw powder into a screw extrusion hydrolysis machine for hydrolysis;

1.6.2 in the hydrolysis process, firstly, a heater is started to heat the machine body by hot water through a coil heat exchanger, and then ingredients are added;

1.6.3 materials enter a spiral extrusion hydrolysis machine, then the flow is controlled to slowly add the 1#, 2# and 3# preparation solutions in the batching storage tank group into the spiral extrusion hydrolysis machine at the same time, and the materials are discharged after thermal insulation and hydrolysis.

2. Straw sulfonation-hydroxymethylation modification method

2.1 weighing a certain amount of straw materials prepared by hydrolysis pretreatment through a 1# aggregate bin weighing device, feeding the weighed straw materials into a reaction unit formed by connecting 1#, 2#, 3# and 4# spiral extruders in series, and carrying out oxidation, sulfonation-hydroxymethylation modification reaction;

2.2 in the modification reaction process, firstly, a heater is started to heat the machine body, so that the materials are heated to about 70 ℃, and then the preparation liquid is sequentially added;

2.3, feeding the material into a No. 1 screw extruder, starting a control valve of a batching storage tank group, slowly adding an oxidant into the No. 1 screw extruder, preserving heat to mix the material, carrying out oxidation chain scission reaction on the straw intrinsic cellulose, and discharging the material into the No. 2 screw extruder after a certain time;

2.4, starting a new round of straw materials to enter a No. 1 screw extruder, and repeating the operation of 2.3 sections to carry out oxidation chain scission reaction;

feeding the 2.51 # spiral extruder into the 2# spiral extruder, adding a sulfonating agent with a certain mass concentration in a 2# batching storage tank, reacting for a certain time, and feeding into the 3# spiral extruder;

2.6 feeding the material into the No. 2 screw extruder by a new round of the No. 1 screw extruder, and repeating the procedure of 2.5 sections to carry out sulfonation modification reaction;

feeding the 2.72 # screw extruder into a 3# screw extruder, adding alkali liquor with a certain concentration dose in a 3# batching storage tank, adjusting the pH value to 8-9, reacting for a certain time, and feeding into a 4# screw extruder;

2.8 feeding the material into a No. 3 screw extruder in a new round of the No. 2 screw extruder, repeating the procedure of 2.7 sections, and adding alkali to adjust the pH value to 8-9;

feeding the 2.93 # screw extruder into a 4# screw extruder, adding a certain mass concentration and a certain dosage of a hydroxymethylation reagent into a 4# batching storage tank, carrying out heat preservation reaction for a certain time, then feeding, weighing by a 2# aggregate bin weighing device, feeding into a storage tank with a trolley, conveying away after reaching a specified weight, and feeding into the next storage tank with the trolley;

2.10 feeding the new 3# screw extruder into the 4# screw extruder, and repeating the procedure of 2.9 to perform hydroxymethylation modification reaction.

All the procedures are completed.

The process flow comprises the following steps of: equipment support, the straw is the garrulous device just, belt cleaning device, drying device in advance, spiral dryer, cyclone, the regrinding device, the little garrulous device of ball mill, 1# collection feed bin weighing device, the screw extrusion machine of hydrolysising, 1# batching storage tank group, 1# heater, 2# collection feed bin weighing device, 2# batching storage tank group, the modified reaction unit is extruded to the spiral, 2# heater, 3# collection feed bin weighing device and the storage tank of taking the shallow are with coarse fodder and powder conveyer belt, above-mentioned part is arranged in proper order by left right side and is settled, link to each other with the conveyer belt between the part.

The invention has the following beneficial effects:

(1) the straw is firstly crushed into straw sections of 1-3 cm by the primary crushing device, and then impurities such as mud and sand in the straw sections are cleaned by the cleaning device, so that the raw materials can be cleaned conveniently, and the problems that the organic components in the straw powder are greatly lost and the subsequent liquid-solid separation is difficult in the cleaning process due to the fact that the straw is crushed too thin are prevented;

(2) the cleaned straw sections are subjected to a drying process of a pre-drying device and a spiral dryer, hot air used by the pre-drying device comes from waste hot air discharged by the spiral dryer, so that the full utilization of energy is realized, the drying efficiency is high, and the level that the moisture content of the straw is below 10% (calculated by mass percent) is easily reached;

(3) by utilizing the characteristics of the ball mill, straw segments of about 1-3 cm are easily finely ground into straw powder of 75-400 mu m, so that the subsequent hydrolysis and the preparation of a water reducing agent are facilitated; after the ball milling treatment, the lignin component in the straws is basically destroyed, and the degradation of the lignin makes the cellulose easier to be hydrolyzed. The crystallinity of the straw is reduced after long-time ball milling, and the ratio of amorphous cellulose and the reaction active area are increased, so that the cellulose of the straw is easier to permeate and hydrolyze by weak acid.

(4) The straw raw material is degraded by a combined organic/inorganic acid mixed acid pretreatment method by spirally extruding by a semi-dry method (the water content in the straw reaches about 10 percent, and liquid-phase hydrolysis catalytic acid is added), and the straw raw material has the advantages of small corrosion to equipment, high degradation rate, simple reaction process, mild reaction conditions, low cost and easy industrial application; and the adverse effects of excessive chloride ions or sulfate ions on the corrosion of the subsequent water reducing agent on concrete and the like caused by only using inorganic acid, hydrochloric acid or sulfuric acid to degrade the straws are avoided or reduced.

(5) The organic acid main catalyst used by the straw raw material pretreated by combining the semidry method screw extrusion with the organic/inorganic acid mixed acid can be used as an unsaturated micromolecule monomer required by the water reducing agent, particularly the unsaturated carboxylic acid micromolecule monomer, and the product performance is not influenced by slight excess;

(6) during the pretreatment of the straw lignocellulose raw material by combining the semidry method screw extrusion with the organic/inorganic acid mixed acid, not only is the straw lignin, the hemicellulose and the cellulose further separated, but also the main products of the straw hydrolysis are mannose, glucose, galactose, xylose andarabinose. Meanwhile, various complex reactions are generated, and some small molecular compounds are generated, for example, hydrolysis sugar, organic acid, furfural, 5-hydroxymethyl furfural, phenolic compounds and the like are usually generated in a pretreated material liquid phase; hemicellulose can concomitantly produce compounds such as acetic acid, arabinose, xylose, mannose, galactose and glucose; cellulose can produce glucose; lignin can produce phenolic compounds; extractives and ashes, etc. can produce wood resins, etc. Meanwhile, part of arabinose and xylose are further hydrolyzed and converted into furfural, mannose and galactose, glucose is further hydrolyzed and converted into hydroxymethyl furfural, furfural is further hydrolyzed and converted into formic acid, and hydroxymethyl furfural is further hydrolyzed and converted into formic acid and levulinic acid. The generated small molecular compounds can be used as small molecular monomers required for synthesizing the water reducing agent, have respective characteristics, such as the retarding and water reducing effects of monosaccharide, polysaccharide and carboxylic acid, the slump retaining effect of furfural and phenolic compounds and the like, and the generated organic weak acid such as formic acid, acetic acid, levulinic acid and the like provides H⁺The method has the advantages of promoting hydrolysis, accelerating hydrolysis process, remarkably promoting degradation of cellulose and lignin in the straws, high saccharification rate, mild reaction conditions, simple reaction process, basically no pollution and easiness in industrial production.

(7) The screw extruder has the advantages of functions of horizontal plug flow, high-speed extrusion and strong shearing, and the functions of high-speed extrusion and strong shearing for a long time further reduce the crystallinity of the straw, and further increase the ratio and the reaction active area of amorphous cellulose, so that the cellulose of the straw is easier to permeate and hydrolyze by weak acid, and the hydrolysis of the straw is more efficient and easy to control. Meanwhile, the shell of the screw extrusion machine body is provided with the coil type heat exchanger, so that the temperature is convenient to rise, the reaction is accelerated, and the operation is easy;

(8) the screw extrusion hydrolysis machine/screw extrusion modification reaction unit is matched with a material preparation storage tank group, so that respective liquid preparation control and step-by-step feeding are facilitated, the screw extrusion modification reaction units are connected in series, the step-by-step control feeding of a modification reagent is facilitated, and an intermittent continuous propulsion operation process is easy to realize.

(9) The batching storage tank group is equipped with simple intercommunication formula level gauge and liquid level scale, is convenient for preliminarily monitor the volume of putting of liquid material, and the liquid discharge pipe disposes precision flowmeter (not drawn), the volume of putting of the accurate control liquid material of being convenient for.

(10) The suspension type weighing and material collecting bin device is convenient to erect on the upper portion of a conveying belt or a storage tank or a reactor, can accurately weigh solid powder, is convenient for accurate feeding of the powder, and ensures the product quality.

In a word, the method and the device prepare the biomass water reducing agent with the water reducing rate of 10-15% by pretreating crop straw raw materials and oxidizing-sulfonating-hydroxymethylating modification of straw lignocellulose, further promote the industrialization process of the low-cost straw-based biomass concrete water reducing agent, and the production device has the characteristics of continuous and compact process, simple equipment, easiness in operation, high straw micro-crushing and hydrolysis efficiency, good modification effect, low cost and easiness in industrialization, and has potential industrial value and application prospect.

Drawings

FIG. 1-flow sheet of the process apparatus of the invention

Detailed Description

In order to make the technical solutions, the creation features, the achievement purposes and the effects of the present invention easy to understand, the specific contents of the present invention are further explained below with reference to the specific embodiments, and the following detailed description is made in conjunction with the accompanying drawings.

Firstly, the characteristics of the straw raw material required by the embodiment are explained for illustration.

The straw raw materials used in the following examples are wheat straw and corn straw harvested in the Tianshui area of Gansu province of 2017, cotton straw harvested in Xinjiang, the harvested straws are air-dried, the dried straws (including the roots, stems and leaves) are pulverized and ground to obtain fine powder, and the fine powder is subjected to composition content analysis and detection of lignin, hemicellulose, cellulose and the like, and the analysis results are shown in the following table 1 (in terms of dry substances, mass fraction%).

TABLE 1 analysis and detection data of straw composition content

(dry basis mass%)

Raw material components%	Cellulose, process for producing the same, and process for producing the same	Hemicellulose	Lignin	Water content ratio	Ash content
						Wheat straw	36.7	27	15.4	5.46	13.1
Corn stalk	38.1	21.1	18.0	6.77	11.5