80results about How to "High degree of sulfonation" patented technology

The invention discloses a sulfomethylated alkali lignin-formaldehyde-sulfonated acetone polymer coal water slurry additive and a preparation method thereof. The additive comprises the following components, by weight, 11.5-20.0 parts of alkali lignin, 4.9-10.0 parts of a sulfonating agent, 0.1-0.8 parts of an alkaline regulator, 4.5-10.0 parts of acetone, 5.4-13.5 parts of formaldehyde, and 47.3-67.2 parts of water. The preparation method comprises the following steps: 1, reacting the alkali lignin with a certain amount of formaldehyde and a certain amount of the sulfonating agent to prepare sulfomethylated alkali lignin; and 2, carrying out a catalytic sulfonation reaction on acetone by the alkaline regulator and the sulfonating agent to obtain a sulfonated acetone prepolymer, adding the prepared sulfomethylated alkali lignin and a formaldehyde solution, and carrying out a polymerization reaction to form the coal water slurry additive containing sulfo, hydroxy and alkyl active groups. So the product and the product stability are improved. The additive of the invention has the advantages of simple method, easily available raw materials, short production period, good stability, nontoxicity, no seasonal and regional restriction of the use, convenient storage and transportation, and realization of the high value utilization of lignin.

This invention discloses a high-performance lignin-based water reducer with high degree of sulfonation and high molecular weight and its preparation method. This water reducer exhibits an excellent water-reducing performance, its water-reducing rate of this lignin-based water reducer reaches 25% at a dosage of 0.70 wt %, which is higher than that of the naphthalene-based water reducer and the sulfonated lignin water reducer prepared by oxidation and sulfonation of alkali lignin, and 28-days compressive strength ratio of the concrete with this water reducer to the concrete without this water reducer is up to 150:100. Furthermore, the water reducer of present invention will not be crystallized in winter, and the concrete iron won't be corroded. The water reducer of the present invention makes the concretes having a low bleeding rate, excellent properties of workability, anti-freeze and anti-carbonization.

The invention discloses a method for preparing sodium lignin sulfonate with high sulfonation degree. A side product, namely wheat straw alkali lignin of a paper-making waste liquid is taken as a main raw material for a free radical degradation reaction under water bath heating conditions under normal pressure at a temperature of between 65 and 75 DEG C, and then an aldehyde substance is dripped to react for 10 to 20 minutes under microwave radiation conditions; and then 50 weight portions of aqueous solution containing 20 to 50 weight portions of sulfonating agent is added into the mixture to react for 1.0 to 2.5 hours under microwave power of between 300 and 1,200W to prepare the sodium lignin sulfonate with higher sulfonation degree. Compared with the prior alkali lignin sulfonation reaction, the technology prepares the sodium lignin sulfonate with high sulfonation degree and water solubility by initiating the degradation of free radicals of lignin, synergistically coordinating microwave radiation effect, using paraformaldehyde to increase active hydroxyl groups in the lignin, increasing the length of an alkyl chain, and then performing a sulfonation reaction, and the sulfonation degree of the sodium lignin sulfonate is higher than 3mmol/g.

The invention discloses a preparation method and an application method of a cellulose xanthogenate heavy metal capturing agent. The preparation method comprises following five steps: cellulose raw material pretreatment, cellulose alkalization, alkalized cellulose sulfonation, sulfonated product transformation reaction, and cellulose xanthogenate purification, wherein in the step of cellulose alkalization, under ice-bath conditions, concentrated alkaline swelling and urea-thiourea mixed solution dissolving are adopted to realize dissolving of cellulose. The alkalization technology is capable of reducing using amount of concentrated alkaline in cellulose alkalization, providing an environment with relatively low alkalinity for subsequent sulfonation, and reducing raw material loss caused by side reaction of carbon disulfide with the alkali in sulfonation process; and at the same time, dissolved cellulose is capable of increasing accessibility of carbon disulfide, and reaction speed of sulfonation. The preparation method possesses following advantages: the prepared cellulose xanthogenate is high in yield, sulfur content, and heavy metal capturing effect; the raw materials are easily available; waste materials high in cellulose content such as bagasse and wood flour can be recycled economically and effectively; using amount of the alkali and carbon disulfide is reduced effectively; and the preparation method possesses high economic cost competitive benefits.

The invention relates to a method for preparing sulfonated polystyrene (strongly acid type) cation exchange resin by taking chlorosulfonic acid as a sulfonating agent. The method has the following characteristics: 1. the advantages of low reaction temperature, short time, less dosage, high sulfonation degree, cost saving, environmental protection and the like can be achieved since chlorosulfonic acid is used as a sulfonating agent; and 2. the sulfonation degree of the resin prepared by using chlorosulfonic acid as a sulfonating agent is controllable in the range of 0.01-95%.

The invention belongs to the technical field of nano-adsorption materials and discloses a preparation method and an application of nano-sulfonated polystyrene microspheres. The preparation method comprises the steps of: adding a styrene monomer, an emulsifier, a buffer agent and an initiator to water, heating the mixture to 68-78 DEG C and performing a reaction for 15-24 h, and washing and drying a solid product to prepare nano polystyrene microspheres; and adding the nano polystyrene microspheres to concentrated sulfuric acid, performing a sulfonation reaction at 20-50 DEG C for 0.5-12 h, and washing and drying a reaction product to obtain the nano-sulfonated polystyrene microspheres. In the method, a sulfonic group is introduced to the surfaces of the polystyrene microspheres so as to prepare the nano-sulfonated polystyrene microspheres. The microspheres have uniform particle size, allows nano-scale self-assembly to form an orderly-arranged array, has high adsorption capacity to heavy metal ions in water, and is high in processing speed.

The invention relates to a preparation method and an application of a hydrophobic starch sulfate ester in a cement water-reducing agent, and belongs to the fields of chemistry and chemical engineering. The preparation method comprises the following steps: adding a sulfamic acid, starch, urea, aliphatic tertiary alcohol or aryl methyl alcohol and water into a reactor under the conditions that the molar ratio of the sulfamic acid to the starch is (0.5-3.0):1, the molar ratio of the urea to the starch is (0.1-3.0):1, the molar ratio of the aliphatic tertiary alcohol or the aryl methyl alcohol to the starch is (0.1-1) and the adding amount of the water accounts for 10% to 30% of the dry weight of the starch; and reacting for 1 to 10 hours at a temperature of 80 DEG C to 150 DEG C, thereby obtaining the hydrophobic starch sulfate ester in which the sulfonyl substitution degree is between 0.04 and 0.89 as well as the alkyl substitution degree is between 0.01 and 0.2. The hydrophobic starch sulfate ester is applied to the cement water-reducing agent, wherein the mass percent of the hydrophobic starch sulfate ester accounts for 0.1% to 1.0% of that of cement. According to the method, a dry method and one-pot reaction are adopted, so that the environmental pollution caused by the application of an organic solvent is avoided. Thus, the production cost is decreased.

The invention relates to a method for preparing modified kraft pulp sodium lignosulphonate. Craft pulp black liquor in paper mill is used as raw material, and CO2 enriched in flue exhaust gas is used as an acid-extracting agent to obtain macromolecular raw lignin by acid extraction. Then the raw lignin is washed in water for removing salt to obtain refined lignin. Finally, the refined lignin is made into the modified kraft pulp sodium lignosulphonate by sulphonation condensation reaction. The preparation method has the characteristics of scientific technology, simple operation, etc. The thermal stability of a product is more than 150 DEG C; the content of inorganic salt is not more than 2 percent; and side product talloel does not exist. In addition, the raw material is the waste liquor of the paper mill, the flue exhaust gas has series pollution and damage effect towards the environment, and the technical proposal produces the macromolecular modified kraft pulp sodium lignosulphonate by the process modification of harmful and exhaust liquor and exhaust gas, so that the invention has high economic value and environmental protection value.

The invention discloses a method for preparing a high-efficiency concrete admixture by using barks rich in tannin, which comprises the following steps: (1) crushing and screening the barks, namely crushing the barks into crushed aggregates of 0.5 to 20 millimeters; (2) leaching and modifying, namely adding water into a leaching pot according to the ratio of solid to liquid of between 1 to 4 and 1 to 6, heating the water and the crushed aggregates and controlling the temperature to between 70 and 120 DEG C, leaching the mixture for 5 to 12 times and 4 to 15 hours step by step by using 4 to 8 normal pressure pot groups, adding a composite modifier consisting of sodium sulfite and sodium bisulfite into the mixture, wherein the adding amount of the composite modifier is 6 to 30 percent of the quality of the barks; and (3) condensing and drying, namely preparing the mixture into powered solid to obtain the high-efficiency concrete admixture. The method not only solves the problem of waste of the barks of trees such as larch, myrica esculenta, black wattle, emblica, coast oak, spruce, eucalyptus, and the like rich in tannin, but also develops a new path for producing a concrete admixture product with high added value by using the barks of the trees such as the larch, the myrica esculenta, the black wattle, the emblica, the coast oak, the spruce, the eucalyptus, and the like.

The invention relates to a multi-cyandiamine monomer and preparation and application thereof, and belongs to the technical field of polymer materials and synthesis thereof. The multi-cyandiamine monomer includes tricyandiamine monomers and tetrocyandiamine monomers. The multi-cyandiamine monomer is polymerized with anhydride to obtain polyimide. Various multi-cyanpolyimide polymers are obtained by chemistry ring-closure and heat ring-closure methods. The polyimide polymer is dissolved in a solvent and a plate coating method is used for paving a film to obtain a desired polyimide film material. The multi-cyanpolyimide material of the invention possesses high thermal stability, excellent film-forming property and excellent adsorbability and dimension stability caused by microscopic intermolecular interaction. The cyan can also be introduced to a sulfonate polyimide material to enhance intermolecular forces between main chains, reduce a swelling coefficient of the sulfonate polyimide material, and enhance dimension stability of the film material which can be used as a proton conduction film material for a fuel cell.

The invention relates to lignin serial coal water slurry dispersing agent and a preparation method thereof, and belongs to the technical field of dispersing agent which is prepared by coal water slurry. The dispersing agent comprises the following raw material components in parts by weight: 1,000 parts of alkali lignin, 20 to 50 parts of polyethylene glycol, 2 to 10 parts of carboxylic acid, 1 to 5 parts of concentrated sulfuric acid, 0.1 to 1 part of hydroquinone, 20 to 60 parts of acrylic acid, 60 to 150 parts of vinyl monomer, 200 to 400 parts of sodium sulfite, 300 to 500 parts of acetaldehyde solution, 30 to 50 parts of oxidant and 10 to 20 parts of reducing agent. Compared with the prior art, the lignin serial coal water slurry dispersing agent adopts the alkali lignin as a raw material, so that the cost is reduced, the average molecular mass of the lignin is remarkably improved, the hydrophily is obviously enhanced, and the dispersing effect is prominently improved; and in addition, the dispersing agent has the advantages of low cost, simple preparation technique, more generality of raw materials, wide sources of the raw materials, cheaper price and good modifying effect; and the resource utilization is implemented for wastes, so that the environmental pollution from the wastes is reduced.

The invention discloses a preparation method of a polysulfone cation-exchange membrane, relating to sulfonated polysulfone. The method comprises the following steps: (1) dissolving 0.65-0.7g of PSF in 48-55mL of N,N-dimethyl acetamide, adding 1.3-1.5mL of chloroethyl isocyanate and 1.3-1.5mL of anhydrous SnCl4, and reacting at 60-70 DEG C for 20-24 hours to obtain a transparent solution; (2) heating the transparent solution to 100 DEG C, adding 5.00-5.50g of sodium 4-hydroxybenzenesulfonate and 0.04-0.05g of dibutyltin dilaurate, reacting for 10-15 hours, adding 200mL of ethanol, separating, and alternately washing with distilled water and ethanol to obtain sulfonated modified polysulfone (PSF-sas); and (3) dissolving the PSF-sas in chloroform, running to form a film, and drying to remove the solvent, thereby obtaining the finished product. The preparation method is simple; and the product has higher degree of sulfonation and cation-exchange membrane properties, and can be used in proton-exchange membrane fuel batteries.

The invention discloses a preparation method for a maleic anhydride esterified starch air-entraining and water-reducing agent. According to the invention, hydrochloric acid is used for acidolysis treatment of starch, so that the molecular chain of the starch is shortened, and the dispersing effect of the water-reducing agent on cement is facilitated; then microwave activation treatment is performed under H2O2 oxidizing conditions, so that hydroxyl groups in the molecular structure of the starch are oxidized into carboxyl groups, and the activity of a sulfonation reaction in a next step is increased, the sulfonation degree of the starch is improved, and the starch has the higher sulfonation degree; finally a part of remaining -OH and maleic anhydride in the starch are subjected to an esterification reaction to release the carboxyl groups, so that the contents of sulfo groups and the carboxyl groups in the prepared starch-based water-reducing agent are increased, the hardness and structural compactness of concrete are improved, and the frost resistance is improved; and besides, the content of hydroxyl groups of retarding groups in molecules of the water reducing agent is effectivelyreduced, the early-stage strength of the concrete is improved, moisture is effectively prevented from penetrating into the concrete, and therefore the water reducing effects and the frost resistance are improved.

The invention relates to a preparation method of hyperbranched sulfonated polyether ether ketone. The preparation method of the hyperbranched sulfonated polyether ether ketone comprises the followingsteps that D1, a sulfonated difluoro benzophenone monomer is prepared, and the difluoro benzophenone monomer is sulfonated to obtain a sulfonated fluorine ketone monomer; D2, the hyperbranched sulfonated polyether ether ketone is prepared, 2,4',6-trifluoro-benzophenone, tetramethyl biphenol, the sulfonated difluoro benzophenone monomer and K2CO3 are matched at the molar ratio of 1:1: (1.5-2):0.4 and dissolved into a DMSO solution, the whole process is carried out under a nitrogen atmosphere, and the hyperbranched sulfonated polyether ether ketone is obtained through drying. According to the preparation method of the hyperbranched sulfonated polyether ether ketone, the sulfonated difluoro benzophenone monomer is adopted, the sulfonated polyether ether ketone is generated, the sulfonation degree can be controlled, the sulfonated polyether ether ketone with the high sulfonation degree is obtained, nucleophilic reaction is used for generating a hyperbranched structure, due to a special three-dimensional space structure of a branched polymer, various performance of the branched polymer and a transmission linear polymer have great difference, and compared with a traditional linear polymer, a three-dimensional space is more stable.

The invention discloses a method for preparing lignin sulfonate by utilizing papermaking black liquid. The method comprises the following steps: S1, preparing raw materials: preparing the raw materials such as the papermaking black liquid, anhydrous sodium sulfite and formaldehyde, wherein the use amount of the sodium sulfite is 2.9 to 3.2 mmol per gram of lignin, the use amount of the formaldehyde is 0.8 to 1.2 mmol per gram of lignin, and the formaldehyde is prepared into a formaldehyde solution; S2, performing reaction: adding the papermaking black liquid into a reaction kettle, adding thesodium sulfite and the formaldehyde solution, stirring and heating, gradually heating to 158 to 165 DEG C, and continuously stirring to perform reaction for 2.5 to 3.5 hours, wherein the consumed timein the heating process is 80 to 100 minutes and the temperature is increased by 1 to 5 DEG C per minute; and S3, discharging: cooling after the reaction, and discharging when the temperature is reduced to 60 to 70 DEG C. The lignin sulfonate prepared by the method has high sulfonation degree and excellent tainting property, dispersibility and heat-resistant stability, has low water content and low content of sulfate, calcium, magnesium, iron, water insoluble matters and total reducing matters, has excellent comprehensive quality and can be widely applied in various fields.

The invention discloses a high molecular weight and moderate sulfonation degree lignin-based pesticide dispersant and its preparation method. The preparation method consists of: first adding a NaOH solution into lignin powder to conduct swelling for 30-60min; adding benzyl chloride, and under the condition of an oil bath at 95-110DEG C, carrying out an etherification reaction for 2-4h; then adding water, sodium lignosulphonate, and a formaldehyde aqueous solution to perform a copolymerization reaction at 80-95DEG C for 1-3h; and adjusting the pH value to 5-9, thus obtaining the high molecular weight and moderate sulfonation degree lignin-based pesticide dispersant. The dispersant prepared in the invention has a weight-average molecular weight of more than 15000 and a sulfonation degree of 0.6-1.0mmol/g, is applicable to 80% dimethomorph water dispersible granules, 80% carbendazim water dispersible granules, 40% myclobutanil wettable powder, and a plurality of pesticide preparations and dosage forms, and has excellent dispersibility, stability, wettability and thermal storage performance.

The invention relates to a method for increasing the sulfonation degree of polyetheretherketone. The method comprises the following steps: mixing polyetheretherketone with a composite sulfonating agent and stirring for reaction at 50 DEG C for 4-8 hours; cooling down to room temperature after the reaction is finished, and pouring the mixed solution into an ice-water mixture for separating out theproduct; washing the resulting product for multiple times with a large amount of pure water until the pH value of the product is neutral, and then subjecting the product to heat treatment for 1-2 hours with heated pure water and carrying out filtering; carrying out drying at 60 DEG C for 12 hours in a drying oven, and then drying at 90 DEG C for 24 hours in a vacuum drying oven to obtain sulfonated polyetheretherketone. The sulfonated polyetheretherketone prepared by the method disclosed in the invention has a high sulfonation degree, which ranges from 50% to 70%, and has excellent film-forming and anti-swelling properties and good mechanical stability; and the preparation process is simple and convenient.