CN114160101A - Resource utilization method of glucosamine production waste residue and application thereof - Google Patents
Resource utilization method of glucosamine production waste residue and application thereof Download PDFInfo
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- CN114160101A CN114160101A CN202111542936.3A CN202111542936A CN114160101A CN 114160101 A CN114160101 A CN 114160101A CN 202111542936 A CN202111542936 A CN 202111542936A CN 114160101 A CN114160101 A CN 114160101A
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- 239000002699 waste material Substances 0.000 title claims abstract description 74
- MSWZFWKMSRAUBD-IVMDWMLBSA-N 2-amino-2-deoxy-D-glucopyranose Chemical compound N[C@H]1C(O)O[C@H](CO)[C@@H](O)[C@@H]1O MSWZFWKMSRAUBD-IVMDWMLBSA-N 0.000 title claims abstract description 61
- MSWZFWKMSRAUBD-UHFFFAOYSA-N beta-D-galactosamine Natural products NC1C(O)OC(CO)C(O)C1O MSWZFWKMSRAUBD-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229960002442 glucosamine Drugs 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000000843 powder Substances 0.000 claims abstract description 74
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 60
- 239000002245 particle Substances 0.000 claims abstract description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000003463 adsorbent Substances 0.000 claims abstract description 34
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 30
- 238000000855 fermentation Methods 0.000 claims abstract description 26
- 230000004151 fermentation Effects 0.000 claims abstract description 26
- 238000005406 washing Methods 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000002243 precursor Substances 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000003763 carbonization Methods 0.000 claims abstract description 20
- 230000000813 microbial effect Effects 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 14
- 238000005550 wet granulation Methods 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 5
- 238000005554 pickling Methods 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims abstract description 4
- 239000000047 product Substances 0.000 claims description 36
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 9
- 230000007935 neutral effect Effects 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 239000000413 hydrolysate Substances 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 229910009819 Ti3C2 Inorganic materials 0.000 claims description 2
- 239000012298 atmosphere Substances 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000004042 decolorization Methods 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 241001052560 Thallis Species 0.000 description 14
- 239000002994 raw material Substances 0.000 description 14
- 239000007788 liquid Substances 0.000 description 10
- 238000001354 calcination Methods 0.000 description 7
- 238000001914 filtration Methods 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 7
- 108010009736 Protein Hydrolysates Proteins 0.000 description 5
- 238000001179 sorption measurement Methods 0.000 description 5
- 239000000049 pigment Substances 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229920002101 Chitin Polymers 0.000 description 1
- 241001391944 Commicarpus scandens Species 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 210000001188 articular cartilage Anatomy 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000004060 metabolic process Effects 0.000 description 1
- 230000007269 microbial metabolism Effects 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 230000035755 proliferation Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 210000001179 synovial fluid Anatomy 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28078—Pore diameter
- B01J20/2808—Pore diameter being less than 2 nm, i.e. micropores or nanopores
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/305—Addition of material, later completely removed, e.g. as result of heat treatment, leaching or washing, e.g. for forming pores
- B01J20/3064—Addition of pore forming agents, e.g. pore inducing or porogenic agents
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H5/00—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium
- C07H5/04—Compounds containing saccharide radicals in which the hetero bonds to oxygen have been replaced by the same number of hetero bonds to halogen, nitrogen, sulfur, selenium, or tellurium to nitrogen
- C07H5/06—Aminosugars
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
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- Chemical Kinetics & Catalysis (AREA)
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- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
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- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Nanotechnology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention relates to the technical field of glucosamine, in particular to a resource utilization method of glucosamine production waste residues and application thereof. The method comprises the following steps: (1) and drying and crushing thallus waste residues generated by preparing glucosamine by a microbial fermentation method to obtain thallus waste residue powder for later use. (2) And uniformly mixing the thallus waste residue powder, calcium carbonate powder and MXene material powder, and then carrying out wet granulation to obtain precursor particles for later use. (3) And carbonizing the precursor particles, pickling the carbonized product after the carbonization treatment, washing the carbonized product with clean water, ethanol and clean water in sequence, and drying to obtain the adsorbent. The process can carbonize and modify the thallus waste residue generated by preparing the glucosamine by the microbial fermentation method to prepare the high-efficiency adsorbent, can be used for decoloring fermentation liquor and reducing chloride ions in subsequent processes, and can improve the quality of a glucosamine finished product.
Description
Technical Field
The invention relates to the technical field of glucosamine, in particular to a resource utilization method of glucosamine production waste residues and application thereof.
Background
Glucosamine is an intermediate for synthesizing articular cartilage and synovial fluid molecules, is an important participant of human metabolism, and currently, China has become the largest world-wide glucosamine producing country. Currently, the method for preparing glucosamine by a microbial fermentation method is a method commonly used by enterprises, and mainly comprises the steps of inoculating microorganisms to a culture medium, carrying out large-scale culture and proliferation by taking glucose as a raw material, carrying out microbial metabolism to generate glucosamine, filtering a fermentation liquid to remove microbial cells, and then carrying out processes of decolorization, purification, concentration, freeze-drying and the like on a filtrate to prepare a glucosamine finished product. Although the microbial fermentation method has the advantages of high conversion efficiency, stable product quality, low production cost and the like, the method has the problem that a large amount of filtered thallus waste residues are difficult to treat, enterprises generally produce a large amount of wet thallus every 1 ton of glucosamine produced by the enterprises, and a large amount of thallus waste residues are usually discarded, buried or burned as garbage every year, so that not only is environmental pollution easily caused, but also resource waste is caused.
Disclosure of Invention
Aiming at the problems, the invention provides a resource utilization method of glucosamine production waste residue and application thereof, the process can carbonize and modify thallus waste residue generated by glucosamine preparation through a microbial fermentation method to prepare a high-efficiency adsorbent, and the high-efficiency adsorbent can be used for decoloring fermentation liquor and reducing chloride ions in subsequent processes, so that the quality of a glucosamine finished product is improved. In order to achieve the purpose, the invention adopts the following technical scheme.
Firstly, a resource utilization method of glucosamine production waste residue is disclosed, which comprises the following steps:
(1) and drying and crushing thallus waste residues generated by preparing glucosamine by a microbial fermentation method to obtain thallus waste residue powder for later use.
(2) And uniformly mixing the thallus waste residue powder, calcium carbonate powder and MXene material powder, and then carrying out wet granulation to obtain precursor particles for later use.
(3) And carbonizing the precursor particles, pickling the carbonized product after the carbonization treatment, washing the carbonized product with clean water, ethanol and clean water in sequence, and drying to obtain the adsorbent.
Further, in the step (1), the thallus waste residue is dried at the temperature of 90-115 ℃ to constant weight, and then is crushed and sieved by a 200-300-mesh sieve, so that thallus waste residue powder is obtained. And the wet thallus is hardened into a whole after passing through the back plate, is made into powder through drying, is convenient to mix with other raw materials, and has higher water content.
Optionally, in the step (2), the particle size of the calcium carbonate powder and the MXene material powder is 150-200 meshes.
Further, in the step (2), the ratio of the thallus waste residue powder to the calcium carbonate powder to the MXene material powder in parts by weight is 1.5-1.8: 0.2-0.35 parts: 0.3 to 0.38 portion. The three are premixed and then subjected to wet granulation, so that precursor particles with thallus waste residue powder as a continuous framework and calcium carbonate powder and MXene material powder as uniformly dispersed phases can be obtained, and a foundation is laid for preparing the adsorbent with a special microstructure and components.
Further, in the step (2), before wet granulation, water accounting for 20-25% of the total mass of the thallus waste residue powder, the calcium carbonate powder and the MXene material powder is added to moisten the powder, or water in corresponding proportion is added according to specific needs to bond the powder, so that wet granulation is performed conveniently.
Further, in the step (2), the MXene material has a general formula of Mn+1XnTxWherein n is 1, 2 or 3, and M represents Ti, V, Mo, Nb and the like; x represents a C or N element, Txrepresents-OH, -O, -F, -Cl, etc. as surface groups. Optionally, the MXene material comprises Ti2CTx、 Ti3C2Tx、Nb2CTx、V2CTx,V4C3Tx、Mo2CTxAnd the like.
Furthermore, in the step (2), the particle size of the precursor particles is preferably controlled to be 2-3 mm, so that the obtained adsorbent has certain mechanical strength, the phenomenon that the adsorbent is easy to break in a collecting process after being used is prevented, the adsorbent is convenient to recycle, and the loss of the adsorbent is reduced.
Further, in the step (3), the temperature of the carbonization treatment is 550-700 ℃, and the time is 1-2 hours. The thallus waste residue can be carbonized through carbonization treatment to form a porous carbon skeleton with good adsorption performance, and the calcium carbonate powder not only serves as an activating agent of the porous carbon skeleton, but also can serve as a pore-foaming agent to be removed in subsequent acid leaching treatment, so that more micropores are manufactured in the adsorbent.
Further, in the step (3), the carbonization treatment is performed in an inert atmosphere or a nitrogen atmosphere.
Further, in the step (3), the acid used in the pickling process includes any one of dilute hydrochloric acid, dilute sulfuric acid, dilute nitric acid, and the like, and the main purpose of the acid is to remove soluble matters such as residual calcium carbonate particles and the like and to produce functional micropores in the adsorbent.
Further, in the step (3), the carbonized product is washed by clean water until the washing liquid is neutral, and then washed by ethanol to remove residual acid liquor, detachable solid debris and the like in the carbonized product.
Secondly, the application of the adsorbent prepared by the resource utilization method of the glucosamine production waste residue in the fields of chemical industry, biology, medical treatment and the like is disclosed, and the adsorbent is preferably used for decoloring glucosamine fermentation liquor obtained by a microbial fermentation method or reducing glucosamine-containing hydrolysate obtained by an acidolysis method and/or reducing chloride ions.
Based on the technical scheme, the invention has the following beneficial effects: the invention takes the thallus waste residue generated by preparing the glucosamine by a microbial fermentation method as a raw material, and prepares the high-efficiency adsorbent by compounding with calcium carbonate powder and MXene materials and then carbonizing and modifying the mixture. The high-efficiency adsorbent prepared by the invention not only contains micropores generated by the carbonization of the thallus waste residue, but also has micropores left by the removal of calcium carbonate powder in the subsequent acid leaching treatment, and the aperture of the micropores is generally larger than that of the micropores generated by the carbonization of the thallus waste residue, namely, the calcium carbonate powder is used as an activating agent of a porous carbon skeleton in the adsorbent and can also be used as a pore-forming agent. The adsorbent can utilize the micropores with small pore diameters generated by the carbonization of the thallus waste residues to adsorb pigment in fermentation liquor, hydrolysate for preparing glucosamine or chloride ions in the hydrolysate, and the micropores with large pore diameters left by removing residual calcium carbonate are convenient for the entry of the fermentation liquor or the hydrolysate, thereby improving the efficient adsorption of the pigment and the chloride ions. Meanwhile, the MXene material is added to remarkably promote the adsorption of chloride ions and the like in the hydrolysate, and the MXene material is of a layered structure with accordion-shaped microscopic characteristics and has huge surface area and abundant surface functional groups, so that the MXene material can quickly adsorb and contain chloride ions, the chloride ions are stably adsorbed in the MXene material, and the MXene material is helpful for more thoroughly removing the chloride ions in the hydrolysate. When the desorption is needed, the adsorbent is boiled by using clean water to separate chloride ions from the adsorbent, and the adsorbent can be recycled after being dried.
Detailed Description
The present invention will be further described by the following specific examples, which are illustrative only and not intended to be limiting, and the scope of the present invention is not limited thereby.
Example 1
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 105 ℃ to constant weight, and then are crushed and sieved by a 250-mesh sieve to obtain waste residues of the thalli for later use.
(2) The thallus waste residue powder, calcium carbonate powder and Ti are mixed2CTxThe powder is prepared from the following raw materials in parts by weight: 0.25 part: 0.35 part of the calcium carbonate powder and the Ti are put into a stirrer to be stirred for 15min to be uniformly mixed2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining for 1.5 hours at 650 ℃ in a nitrogen atmosphere for carbonization treatment, immersing the obtained carbonized product into 1mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 2
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 115 ℃ to constant weight, and then are crushed and sieved by a 250-mesh sieve to obtain waste residues of the thalli for later use.
(2) The thallus waste residue powder, calcium carbonate powder and Nb are added2CTxThe powder is prepared from the following components in parts by weight: 0.20 part: 0.30 part of the raw materials are put into a stirrer to be stirred for 15min to be uniformly mixed, and the calcium carbonate powder and the Nb powder are2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining for 1.0 hour at 700 ℃ in a nitrogen atmosphere for carbonization, immersing the obtained carbonized product into 1mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 3
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 90 ℃ to constant weight, and then are crushed and sieved by a 300-mesh sieve to obtain the waste residues of the thalli for later use.
(2) Mixing the thallus waste residue powder, calcium carbonate powder and V2CTxThe powder is prepared from the following components in parts by weight: 0.35 parts of: 0.38 portion of the calcium carbonate powder and V are put into a stirrer to be stirred for 15min to be uniformly mixed2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining at 550 ℃ for 2.0 hours in a nitrogen atmosphere for carbonization treatment, immersing the obtained carbonized product in 1.5mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 4
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 100 ℃ to constant weight, and then are crushed and sieved by a 200-mesh sieve to obtain the waste residues of the thalli for later use.
(2) The thallus waste residue powder, calcium carbonate powder and Mo2CTxThe powder is prepared from the following components in parts by weight: 0.30 parts of: 0.36 part of the mixture is placed in a stirrer to be stirred for 15min so that the calcium carbonate powder and the Mo are uniformly mixed2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining at 650 ℃ in a nitrogen atmosphere for 2.0 hours for carbonization, immersing the obtained carbonized product in 1.5mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 5
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 105 ℃ to constant weight, and then are crushed and sieved by a 250-mesh sieve to obtain waste residues of the thalli for later use.
(2) Mixing the thallus waste residue powder and Ti2CTxThe powder is prepared from the following raw materials in parts by weight: 0.25 part of Ti is put into a stirrer to be stirred for 15min to be uniformly mixed with the three2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining for 1.5 hours at 650 ℃ in a nitrogen atmosphere for carbonization treatment, immersing the obtained carbonized product into 1mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 6
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 105 ℃ to constant weight, and then are crushed and sieved by a 250-mesh sieve to obtain waste residues of the thalli for later use.
(2) 1.6 parts of the thallus waste residue powder and calcium carbonate powder by weight: 0.25 part of the calcium carbonate powder is placed in a stirrer to be stirred for 15min so as to be uniformly mixed, and the particle size of the calcium carbonate powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining for 1.5 hours at 650 ℃ in a nitrogen atmosphere for carbonization treatment, immersing the obtained carbonized product into 1mol/L hydrochloric acid until no bubbles emerge, and filtering to separate the carbonized product.
(4) Washing the carbonized product obtained in the step (3) with clear water until the washing liquid is neutral, then washing the carbonized product with ethanol and clear water in sequence, and then drying at 50 ℃ to constant weight to obtain the adsorbent.
Example 7
A resource utilization method of glucosamine production waste residue comprises the following steps:
(1) the waste residues of the thalli generated by preparing glucosamine by a microbial fermentation method are dried at 105 ℃ to constant weight, and then are crushed and sieved by a 250-mesh sieve to obtain waste residues of the thalli for later use.
(2) The thallus waste residue powder, calcium carbonate powder and Ti are mixed2CTxThe powder is prepared from the following raw materials in parts by weight: 0.25 part: 0.35 part of the calcium carbonate powder and the Ti are put into a stirrer to be stirred for 15min to be uniformly mixed2CTxThe particle size of the powder is 150-200 meshes. And then adding water to wet the raw materials for wet granulation to obtain precursor particles with the particle size of 2-3 mm for later use.
(3) And placing the precursor particles in a tubular heating rate, calcining for 1.5 hours at 650 ℃ in a nitrogen atmosphere for carbonization, washing the carbonized product with clear water after the carbonization is finished, then washing the carbonized product with ethanol and clear water in sequence, and drying at 50 ℃ to constant weight to obtain the adsorbent.
The adsorbent obtained in the above embodiment is used for performing a chloride ion removal test on glucosamine, wherein the glucosamine is prepared by hydrolyzing chitin with concentrated hydrochloric acid, and contains partial chloride ions. The glucosamine was dissolved in water before the test, the chloride ion concentration of the glucosamine solution obtained by the test was 0.103g/mL, seven portions of the glucosamine solution were taken and added to the adsorbents prepared in the above examples 1 to 7 at a ratio of 2g/mL, and the chloride ion concentration of the glucosamine solution was measured after adsorption, and the results are shown in table 1.
TABLE 1
Example number | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
After adsorbent treatment (g/mL) | 0.041 | 0.027 | 0.033 | 0.038 | 0.077 | 0.84 | 0.094 |
It can be seen that the preparation examples of examples 1 to 4 have a good effect of removing chloride ions from the glucosamine solution, and the preparation examples of examples 5 to 7 have a weak ability of removing chloride ions from the glucosamine solution, because the adsorbent prepared in examples 1 to 4 can utilize the small-pore-diameter micropores generated by the carbonization of the waste residues of the thallus to adsorb the pigment in the fermentation liquid, the hydrolysate for preparing the glucosamine, or the chloride ions in the hydrolysate, and the large-pore-diameter micropores left by removing the residual calcium carbonate facilitate the entry of the fermentation liquid or the hydrolysate, thereby improving the efficient adsorption of the pigment and the chloride ions. Meanwhile, the special microstructure of the MXene material can be used for quickly adsorbing and containing chloride ions, so that the chloride ions are stably adsorbed in the MXene material, and the removal of the chloride ions in the hydrolysate is facilitated more thoroughly.
Finally, it should be understood that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. While the embodiments of the present invention have been described, it is not intended to limit the scope of the present invention, and it will be apparent to those skilled in the art that various modifications and variations can be made without inventive faculty based on the technical solutions of the present invention.
Claims (10)
1. A resource utilization method of glucosamine production waste residue is characterized by comprising the following steps:
(1) drying and crushing thallus waste residues generated by preparing glucosamine by a microbial fermentation method to obtain thallus waste residue powder for later use;
(2) uniformly mixing the thallus waste residue powder, calcium carbonate powder and MXene material powder, and then carrying out wet granulation to obtain precursor particles for later use;
(3) and carbonizing the precursor particles, pickling the carbonized product after the carbonization treatment, washing the carbonized product with clean water, ethanol and clean water in sequence, and drying to obtain the adsorbent.
2. The resource utilization method of glucosamine production waste residue according to claim 1, wherein in the step (1), the thallus waste residue is dried at 90-115 ℃ to constant weight, and then is crushed and sieved by a 200-300 mesh sieve to obtain thallus waste residue powder; preferably, in the step (2), the particle size of the calcium carbonate powder and the MXene material powder is 150-200 meshes.
3. The resource utilization method of glucosamine production waste residue according to claim 1, wherein in the step (2), the weight ratio of the thallus waste residue powder, the calcium carbonate powder and the MXene material powder is 1.5-1.8: 0.2-0.35 parts: 0.3 to 0.38 portion.
4. The resource utilization method of glucosamine production waste residue as claimed in claim 1, wherein in the step (2), the MXene material has a general formula of Mn+1XnTxWherein n is 1, 2 or 3, and M represents Ti, V, Mo or Nb; x represents a C or N element, TxRepresents a surface group-OH, -O, -F, -Cl; preferably, the MXene material comprises Ti2CTx、Ti3C2Tx、Nb2CTx、V2CTx,V4C3Tx、Mo2CTxAt least one of (1).
5. The resource utilization method of glucosamine production waste residue as claimed in claim 1, wherein in the step (2), water with the total mass of 20-25% of the thallus waste residue powder, the calcium carbonate powder and the MXene material powder is added to moisten the powder before wet granulation.
6. The resource utilization method of glucosamine production waste residue as recited in claim 1, wherein in step (2), the particle size of the precursor particles is controlled to be 2-3 mm.
7. The resource utilization method of glucosamine production waste residue as claimed in claim 1, wherein in step (3), the temperature of the carbonization treatment is 550-700 ℃ and the time is 1-2 hours; preferably, the carbonization treatment is performed in an inert atmosphere or a nitrogen atmosphere.
8. The resource utilization method of glucosamine production waste residue as recited in claim 1, wherein in step (3), the acid used in the pickling treatment comprises any one of dilute hydrochloric acid, dilute sulfuric acid and dilute nitric acid.
9. The resource utilization method of glucosamine production waste residue according to any one of claims 1 to 8, wherein in the step (3), the carbonized product is washed with clean water until the washing solution is neutral, and then washed with ethanol.
10. The use of the adsorbent prepared by the resource utilization method of glucosamine production waste residue according to any one of claims 1 to 9 in the fields of chemical industry, biology and medical treatment, preferably in the decolorization and/or chloride ion reduction of glucosamine fermentation broth obtained by microbial fermentation or glucosamine-containing hydrolysate obtained by acidolysis.
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