CN111713499A - Synthesis method of biological sugar multi-ionic liquid - Google Patents
Synthesis method of biological sugar multi-ionic liquid Download PDFInfo
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Abstract
The invention discloses a method for synthesizing biological sugar multi-element ionic liquid, which comprises the steps of sequentially and quantitatively adding tap water, acetic acid, boric acid and zinc sulfate into a reaction kettle according to the sequence of steps, starting stirring until a completely dissolved transparent solution is obtained, directly and quantitatively adding phosphoric acid into the reaction kettle, quantitatively and slowly adding hydrochloric acid, quantitatively and dropwise adding sulfuric acid, quantitatively and dropwise adding nitric acid, after the temperature of all the acid is stabilized, heating to 70 ℃, quantitatively and quickly adding treated chitosan, heating to 80 ℃, keeping the temperature at 80 +/-2 ℃ for reaction for four hours, cooling to 20 ℃, adding hydrogen peroxide, uniformly mixing and discharging, wherein the ionic liquid has the excellent performance of the developed chemical ionic liquid in a green chemical framework, simultaneously has the physicochemical properties and functions of chitosan oligosaccharide, obtains human and animal excrement and kitchen garbage source treatment through molecular structure design, realizes the special functions of humanization, sanitation, harmlessness and resource utilization of the source.
Description
Technical Field
The invention relates to the technical field of functional ionic liquid based on biosaccharide synthesis, in particular to a biosaccharide multi-ionic liquid synthesis method.
Background
The ionic liquid is a brand new composite and functional material developed under the green chemical framework in the late 90 s, the ionic liquid is a liquid electrolyte completely consisting of ions, and the ionic liquid has many excellent properties, such as complete liquid state temperature distribution, almost no vapor pressure, no volatilization, no flammability, wide electrochemical window, good dissolving capacity and reaction catalyst effect on organic matters, inorganic matters and high polymer inorganic matters, and the unique physical and chemical properties and functional effects of the ionic liquid cause great attention to academia and industry, and the research and application fields of the ionic liquid are continuously expanded.
After 2000, with the continuous and intensive research of science and technology workers, the physicochemical properties of ionic liquids become adjustable, such as: fluidity, conductivity, liquid range; chemical properties, such as: the polarity, acidity, chirality, coordination ability, chemical stability and solubility can be adjusted according to the need, and special functions can be obtained through molecular design.
The chemical ionic liquid is a molten salt system consisting of cations and inorganic anions, the types of the ionic liquid are more than 1018 according to different arrangement and combination modes of the cations and the anions, and the ionic liquid which is actually used at present is mainly divided into four types, namely imidazoles, pyridines, quaternary ammonium salts and quaternary phosphonium salts. Dialkyl imidazoles are the most commonly used ionic liquids because of their ease of synthesis and their stable nature, and the ionic liquids can be classified into two categories according to the difference of anions: one is halide salt + ACH3 (or ACBr3) ionic liquids. The ionic liquid is researched earlier, and the biggest defect is that the ionic liquid is extremely sensitive to water, and needs to be operated and used under vacuum or inert atmosphere, so that the research and the application of the ionic liquid are greatly limited. Another class of ionic liquids is the one found in 1992 to have a melting point of 12 ℃ [ C2mim】【BF4Developed on the basis of ionic liquids. It is different from ACH3The ionic liquid of the type, the composition of which is fixed and can stably exist in water and air, is the most studied ionic liquid in recent years, the cations of the ionic liquid are still the five types, and the anions are mainly; [ BF ]4】-,【BF6】-,【CF3SO4】-,【(CF3SO2)2N】-,【C3F7COO】-,【C4F9SO3】-,【CF3COO】-,【(CF3SO2)3C】-,【(C2F5SO2)3C】-,【(C2F5SO2)2N】-,【SbF6】-,【AsF6】-,【NO2】【NO3】-And the like.
At present, although the chemical ionic liquids are considered as 'green solvents', after the chemical ionic liquids enter the environment, certain toxicity still exists, therefore, when the ionic liquid is developed and utilized, the related researches such as the recycling of the related ionic liquid, the ecotoxicology, the degradation treatment technology and the like are required to be enhanced, the secondary pollution to the environment is ensured not to be caused, meanwhile, the chemical ionic liquid is difficult to separate from the treated substances for recycling, the high production cost is a key problem restricting the application and popularization of the chemical ionic liquid with excellent performance, the source treatment of human and animal excrements and kitchen garbage is acknowledged at home and abroad, the humanization, the sanitation and the harmlessness are realized, and the resource is the development trend and the direction of the domestic sewage treatment, however, the function of the chemical ionic liquid cannot meet the requirement, so there is a need to develop a new biological conversion ecological ionic liquid, i.e. the biological sugar multi-ionic liquid of the present invention.
Disclosure of Invention
The invention aims to provide a method for synthesizing biological sugar multi-component ionic liquid, which adopts the biological sugar multi-component ionic liquid synthesized by a one-step method and can completely overcome the problems existing in chemical ionic liquid, and the invention realizes the performance requirements of quaternization on the ionic liquid according to the source treatment of human and animal excrements and kitchen garbage, realizes the special functions obtained by molecular design, is a miniaturized and automatic cleaning process design for the source treatment equipment of the human and animal excrements and the kitchen garbage, and overcomes the dependence on the functional materials: a novel biological sugar multi-ionic liquid solution fills the gap of ionic liquid research and development at home and abroad, and solves the problems in the background technology.
The invention aims to provide a synthesis technology of biomass multi-element ionic liquid, which solves the problems of the chemical ionic liquid and the problem that the chemical ionic liquid cannot be applied to the source treatment of kitchen waste of human and livestock excrements to realize the quaternization.
The biological sugar multi-element ionic liquid is a technology for synthesizing the biological sugar multi-element ionic liquid in one step by utilizing a third-generation biological technology called by the international scientific and technological community after gene engineering and protein engineering and degrading chitosan into chitosan oligosaccharide, taking chitosan oligosaccharide which is the only biomass with positive charges in the nature as a cation and anions provided by various inorganic acids.
In order to achieve the purpose, the invention provides the following technical scheme: a method for synthesizing biological sugar multi-ionic liquid comprises the following steps:
the method comprises the following steps: firstly, putting tap water into a reaction kettle according to 63 percent of the total feeding amount;
step two: weighing acetic acid according to 1.4% of the total feeding amount and putting into a reaction kettle;
step three: starting stirring, weighing and adding boric acid into a reaction kettle according to 1.3 percent of the total feeding amount, weighing and adding zinc sulfate into the reaction kettle according to 1.6 percent of the total feeding amount, and completely dissolving the zinc borate sulfate into a transparent solution at normal temperature;
step four: weighing phosphoric acid according to 8.5 percent of the total feeding amount, continuously adding the phosphoric acid into a reaction kettle, slowly adding hydrochloric acid into the reaction kettle, wherein the feeding speed is preferably no white smoke, dropwise adding sulfuric acid after the addition is finished, controlling the dropwise adding speed to be no white smoke, slowly raising the temperature, controlling the temperature rise from dropwise adding to sulfuric acid after the addition to be no more than 40 ℃, dropwise adding nitric acid after the addition of sulfuric acid is finished, wherein the heat effect is not obvious, and the dropwise adding speed can be higher;
step five: stirring for ten minutes after the nitric acid is added, after the temperature is stabilized, heating to 70 ℃, and weighing and adding the cleaned, dried and crushed chitosan according to 3.9 percent of the total feeding amount;
step six: keeping the temperature at 80 +/-2 ℃ for reaction for four hours, and then cooling;
step seven: adding hydrogen peroxide when the prepared biomass multi-element ionic liquid is cooled to 20 ℃ according to the mass ratio of the total inventory of the inorganic acid to the hydrogen peroxide of 7: 3.
Preferably, the concentration of acetic acid in the second step is more than or equal to 98 percent.
Preferably, the concentration of boric acid in step three is 99%.
Preferably, the concentration of zinc sulfate in the third step is 98%.
Preferably, the concentration of phosphoric acid in the fourth step is 85%.
Preferably, the concentration of hydrochloric acid in the step four is 30%.
Preferably, the concentration of sulfuric acid in the fourth step is 98%.
Preferably, the concentration of nitric acid in the fourth step is 68%.
Preferably, the purity D.D of the chitosan in the fifth step is more than or equal to 90 percent.
Preferably, the content of the hydrogen peroxide in the seventh step is 30%.
Compared with the prior art, the invention has the beneficial effects that:
the ionic liquid has the excellent performance of the developed chemical ionic liquid in a green chemical framework, the requirements of the four-purpose (humanization, sanitation, harmlessness and recycling) on the performance of the ionic liquid are realized aiming at the source treatment of human and animal excrements and kitchen garbage, the special functions are obtained through molecular design, and the ionic liquid overcomes the dependence of the supported key technology and makes a great contribution to the construction of whitening villages and towns and the ecological civilization construction and economic construction of the country.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Figure 2 is a representation of the ingredients of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, the present invention provides a technical solution: a method for synthesizing biological sugar multi-ionic liquid comprises the following steps:
the method comprises the following steps: firstly, putting tap water (1) into a reaction kettle according to 63 percent of the total feeding amount;
step two: weighing acetic acid (2) according to 1.4 percent of the total feeding amount and putting into a reaction kettle;
step three: starting stirring, weighing and adding boric acid (3) into a reaction kettle according to 1.3 percent of the total feeding amount, weighing and adding zinc sulfate (4) into the reaction kettle according to 1.6 percent of the total feeding amount, and completely dissolving the boric acid (3) and the zinc sulfate (4) into a transparent solution at normal temperature;
step four: the phosphoric acid (5) is weighed according to 8.5 percent of the total feeding amount and is continuously added into a reaction kettle, then the hydrochloric acid (6) is slowly added into the reaction kettle, the feeding speed is suitable for not generating white smoke, after the addition is finished, the sulfuric acid (7) is dropwise added, the dropwise adding speed is controlled not to generate white smoke, the temperature rise is slow, the temperature rise of the sulfuric acid is controlled not to exceed 40 ℃ from the dropwise addition to the completion of the addition, the nitric acid (8) is dropwise added after the sulfuric acid is completely added, the heat effect is not obvious, and the dropwise adding speed can be higher;
step five: stirring for ten minutes after the nitric acid (8) is added, and weighing and adding the cleaned, dried and crushed chitosan (9) according to 3.9 percent of the total feeding amount when the temperature is raised to 70 ℃ after the temperature is stabilized;
step six: keeping the temperature at 80 +/-2 ℃ for reaction for four hours, and then cooling;
step seven: adding hydrogen peroxide (10) when the temperature of the prepared biomass multi-element ionic liquid is reduced to 20 ℃ according to the mass ratio of the total inventory of the inorganic acid to the hydrogen peroxide of 7: 3.
Wherein, the tap water (1) is domestic water; the concentration of the acetic acid (2) is more than or equal to 98 percent; the concentration of boric acid (3) is 99%; the concentration of zinc sulfate (4) is 98 percent; the concentration of phosphoric acid (5) is 85%; the concentration of hydrochloric acid (6) is 30%; the concentration of sulfuric acid (7) is 98%; the concentration of nitric acid (8) is 68%; the purity D.D of the chitosan (9) is more than or equal to 90 percent; the content of the hydrogen peroxide (10) is 30 percent.
The biomass multi-element ionic liquid prepared by the steps can be divided into two layers at 50 ℃, the upper layer solution can contain components of micromolecule water-soluble biomass multi-element ionic liquid and a large amount of H+The cleaning and disinfecting liquid can replace water to convey human and animal excrement and kitchen garbage, not only increases the fluidity, but also does not form scale, so that the pipeline of the treatment equipment is cleaned, and the biological multi-element ionic liquid for killing the solid in the harmful bacteria, viruses, parasites, parasitic ova, human and animal excrement and kitchen garbage can be added in the cleaning and disinfecting liquidThe organic matters in the human and animal excreta are decomposed into carbon dioxide and water as a solvent and a catalyst for reaction, the inorganic matters are adsorbed, combined and coprecipitated by ionic liquid, and can be completely solidified and separated out when the temperature is reduced to 50 ℃, so that the nutrients are continuously increased each time the nutrient is used, and the nutrient can be repeatedly recycled for countless times.
The invention relates to biose polybasic ionic liquid synthesized by a one-step method, which is innovative ionic liquid prepared by degrading chitosan oligosaccharide which is the only existing biomass chitosan with positive charge in the nature into cation, using 5 inorganic acids such as hydrochloric acid, phosphoric acid, sulfuric acid, nitric acid, boric acid and the like and polybasic anion provided by inorganic acid salt of zinc in 2 percent acetic acid solution, and simultaneously carrying out chitosan degradation and anion combination reaction in one step.
The ionic liquid has the excellent performance of the developed chemical ionic liquid in a green chemical framework, the requirements of the four-purpose (humanization, sanitation, harmlessness and recycling) on the performance of the ionic liquid are realized aiming at the source treatment of human and animal excrements and kitchen garbage, the special functions are obtained through molecular design, and the ionic liquid overcomes the dependence of the supported key technology and makes a great contribution to the construction of whitening villages and towns and the ecological civilization construction and economic construction of the country.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (10)
1. A method for synthesizing biological sugar multi-ionic liquid is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: firstly, putting tap water (1) into a reaction kettle according to 63 percent of the total feeding amount;
step two: weighing acetic acid (2) according to 1.4 percent of the total feeding amount and putting into a reaction kettle;
step three: starting stirring, weighing and adding boric acid (3) into a reaction kettle according to 1.3 percent of the total feeding amount, weighing and adding zinc sulfate (4) into the reaction kettle according to 1.6 percent of the total feeding amount, and completely dissolving the boric acid (3) and the zinc sulfate (4) into a transparent solution at normal temperature;
step four: the phosphoric acid (5) is weighed according to 8.5 percent of the total feeding amount and is continuously added into a reaction kettle, then the hydrochloric acid (6) is slowly added into the reaction kettle, the feeding speed is suitable for not generating white smoke, after the addition is finished, the sulfuric acid (7) is dropwise added, the dropwise adding speed is controlled not to generate white smoke, the temperature rise is slow, the temperature rise of the sulfuric acid is controlled not to exceed 40 ℃ from the dropwise addition to the completion of the addition, the nitric acid (8) is dropwise added after the sulfuric acid is completely added, the heat effect is not obvious, and the dropwise adding speed can be higher;
step five: stirring for ten minutes after the nitric acid (8) is added, and weighing and adding the cleaned, dried and crushed chitosan (9) according to 3.9 percent of the total feeding amount when the temperature is raised to 70 ℃ after the temperature is stabilized;
step six: keeping the temperature at 80 +/-2 ℃ for reaction for four hours, and then cooling;
step seven: adding hydrogen peroxide (10) when the temperature of the prepared biomass multi-element ionic liquid is reduced to 20 ℃ according to the mass ratio of the total inventory of the inorganic acid to the hydrogen peroxide of 7: 3.
2. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: and in the second step, the concentration of the acetic acid (2) is more than or equal to 98 percent.
3. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of boric acid (3) in step three is 99%.
4. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of zinc sulfate (4) in the third step is 98%.
5. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of phosphoric acid (5) in the fourth step is 85%.
6. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of the hydrochloric acid (6) in the fourth step is 30 percent.
7. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of the sulfuric acid (7) in the fourth step is 98%.
8. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the concentration of nitric acid (8) in the fourth step is 68%.
9. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: and in the fifth step, the purity D.D of the chitosan (9) is more than or equal to 90 percent.
10. The method for synthesizing biological sugar multi-ionic liquid according to claim 1, which is characterized in that: the content of the hydrogen peroxide (10) in the seventh step is 30 percent.
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CN103875666A (en) * | 2012-12-19 | 2014-06-25 | 魏亚中 | Degerming composition and application thereof |
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CN109452318A (en) * | 2018-11-14 | 2019-03-12 | 湖北科田药业有限公司 | A kind of persistent disinfectant |
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CN1803771A (en) * | 2006-01-23 | 2006-07-19 | 周新基 | Method for preparing peroxy acetic acid |
CN101891904A (en) * | 2010-06-23 | 2010-11-24 | 中国农业科学院植物保护研究所 | Kelp oligosaccharide and preparation method and application thereof |
CN103875666A (en) * | 2012-12-19 | 2014-06-25 | 魏亚中 | Degerming composition and application thereof |
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