CN101288846A - Method for preprocessing and producing rice hull ash adsorbent using with microbe - Google Patents
Method for preprocessing and producing rice hull ash adsorbent using with microbe Download PDFInfo
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- CN101288846A CN101288846A CNA2008101006353A CN200810100635A CN101288846A CN 101288846 A CN101288846 A CN 101288846A CN A2008101006353 A CNA2008101006353 A CN A2008101006353A CN 200810100635 A CN200810100635 A CN 200810100635A CN 101288846 A CN101288846 A CN 101288846A
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- rice hull
- rice
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Abstract
The invention discloses a method for producing rice husk ash adsorbent by micro-organism pre-disposal. Firstly, the rice husk is pre-disposed by a two-step method, namely, the surface performance of the rice husk is improved by cellulase production and lignin enzyme micro-organism; the rice husk ash is then fabricated by distillation; the rice husk ash is then activated and dried to gain the rice husk ach adsorbent. The method of the invention adopts the micro-organism to improve the surface performance of the rice husk so as to produce the rice husk ash adsorbent; the adsorbent has obvious effects on the decoloration of grease pigment and greatly improves the development value of the rice husk industry.
Description
Technical field
The present invention relates to the production method of rice hull ash adsorbent using, be specifically related to a kind of method of preprocessing and producing rice hull ash adsorbent using with microbe.
Background technology
Rice husk is the processed side product of rice-hulling mill, itself is worth not highly, has made discarded object in the processing of rural area.And modern science and technology prove, rice husk is rich in cellulose, pentosan, lignin, ash and grades, and has the physical attribute that proportion is little, thermal conductivity factor is low, industrial wide development value are arranged.China is large agricultural country, produces the about 250Mt of paddy per year, and the about 50Mt of processing rice husk accounts for 20% of paddy gross output.
Rice husk is widely used, and developmental research both at home and abroad is very popular.The main method of processing and utilization rice husk and approach are to make adsorbent, as the poisonous element in the metal ion in the adsorbent solution, adsorbed water or the gas, the carrier as enzyme, the coloring agent in the adsorbent solution; Adopt method production chemical products such as high temperature method, acid and alkali hydrolysis method; Produce biologic product; Be applied to plant husbandry with improve the soil, improve output, improve the ventilation condition of soil and water holding condition, as covering with prevent certain micro-organisms infringement crop, as lignocellulosic substance, be used for planting some special crop etc.
Formed having of industry at home: produce silica, carborundum, waterglass, active carbon, use rice husk power generating, produce furfural etc. with rice husk.Established abroad industry has: the rice husk coating of the rice-hull cement of the rice husk brick of Japan, the rice husk lightweight concrete of the U.S., Korea S, the rice husk waterproof material of India, the U.S., the rice husk insulating firebrick of Brazil.
China utilizes the rice husk level lower, at some enterprise's rice husk even become big pollution sources.Therefore, how utilizing rice husk fully, make its increment, then is a sizable problem.
Research as fat decolourizing agent also has much for rice husk, but all only be confined to processing procedure research to the physics or the chemistry of charring rice husk, and adopt microorganism earlier rice husk to be carried out preliminary treatment, thereby and then carry out operations such as destructive distillation, activation and make rice hull ash still blank at home and abroad the research that the absorption property of grease pigment improves greatly.
Summary of the invention
The objective of the invention is to: a kind of method of preprocessing and producing rice hull ash adsorbent using with microbe is provided, adopts the regeneration of microbial pretreatment rice husk to produce rice hull ash adsorbent using earlier, improve the absorption property of rice hull ash adsorbent using the grease pigment.
Technical solution of the present invention is: this method at first adopts two-step method that rice husk is carried out preliminary treatment, promptly improve the rice husk surface nature by cellulase-producing and product lignoenzyme microorganism, rice hull ash is made in destructive distillation then, again to rice hull ash activate, dry rice hull ash adsorbent using.
Production method of the present invention comprises following concrete steps:
The first step, cellulase-producing microbial degradation rice husk, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, degradation time 50-130 hour, 25 ℃-37 ℃ of degradation temperatures, microorganism in the cellulase-producing nutrient solution is aspergillus niger, Trichoderma viride, koning trichoderma, trichoderma reesei, bacillus subtilis, bacillus licheniformis or wax sample bud bacillus, and its spore or cell concentration are 10
7-10
8Cfu/ml;
Second step, produce lignoenzyme microbial fermentation rice husk, ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, fermentation time 210-300 hour, fermentation temperature 25-30 ℃, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, and its spore concentration is 10
7-10
8Cfu/ml;
In the 3rd step, the rice husk that ferments is dry to be handled, and baking temperature 80-100 ℃, rice husk moisture content 8-12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, and water smoking temperature 120-140 ℃, time 30-60 minute; 260-280 ℃ of pre-charing phase temperature, time 30-60 minute; 450-500 ℃ of charing phase temperature, time 45-75 minute; 600-650 ℃ of calcination stage temperature, time 90-120 minute;
The 5th step, the rice hull ash activation processing, per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, and at 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, adsorbent moisture is 8%.
In the method for preprocessing and producing rice hull ash adsorbent using with microbe of the present invention, the aspergillus niger nutrient solution is by adding cellulose powder 5g, potassium nitrate 30g, polyethylene glycol 1g in every premium on currency, pH6.5, and inserting 50-100ml concentration is 10
7-10
8The aspergillus niger spore suspension of cfu/ml, 32 ℃ of cultivation temperature, incubation time 130 hours.
In the method for preprocessing and producing rice hull ash adsorbent using with microbe of the present invention, Trichoderma viride, koning trichoderma nutrient solution are by adding 2g (NH in every premium on currency
4)
2HPO
4, 0.0044g ZnSO
47H
2O, 0.2g K
2HPO
4, 0.001g MnSO
44H
2O, 0.8g KH
2PO
4, 0.005g FeSO
4, 0.9gMgSO
47H
2O, 0.005g Triammonium citrate, 2g peptone, 1g yeast extract, 0.001g/LV
B1, inserting 50-100ml concentration is 10
7-10
8The spore suspension of cfu/ml Trichoderma viride or koning trichoderma, 28 ℃ of cultivation temperature were cultivated 96 hours.
In the method for preprocessing and producing rice hull ash adsorbent using with microbe of the present invention, the trichoderma reesei nutrient solution is by adding 10g (NH in every premium on currency
4)
2SO
4, 0.5g CaCl
2, 3g KH
2PO
4, 1gMgSO
47H
2O, inserting 50-100ml concentration is 10
7-10
8Cfu/ml trichoderma reesei spore suspension, 28 ℃ of cultivation temperature were cultivated 96 hours.
In the method for preprocessing and producing rice hull ash adsorbent using with microbe of the present invention, bacillus subtilis, bacillus licheniformis, bacillus cereus nutrient solution are by add 2g corn flour, 0.3g beef extract, 0.2g peptone, 0.5g NaCl, 0.1g KH in every premium on currency
2PO
4, 0.1gNa
2HPO
4, 0.05g MgSO
4, pH value 7.0, inserting 50-100ml concentration is 10
7-10
8The bacillus subtilis of cfu/ml, bacillus licheniformis, bacillus cereus suspension, 37 ℃ of cultivation temperature were cultivated 56 hours.
In the method for preprocessing and producing rice hull ash adsorbent using with microbe of the present invention, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2g Na
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 50-100ml concentration is 10
7-10
8Cfu/ml whiterot fungi spore suspension, was cultivated 210-300 hour by cultivation temperature 25-30 ℃.
With the rice hull ash adsorbent using that makes with 1% addition and commercial grease decolorizer product atlapulgite respectively with 1%, 2%, 3% addition and the rice hull ash that makes without microbiological treatment are carried out the grease-decolor experiment with 2% addition, crude oil is that soybean oil mixes (w/w) with No. six solvents with 20% ratio, the grease that under the 350-550nm wavelength, decolours scanning, measure absorbance, increase along with addition, absorbance is on a declining curve, find when adding 1% product volume, its result sees that than 3% atlapulgite and 2% not bad without the additive effect of the rice hull ash of microbial pretreatment figure is as follows:
The present invention produces rice hull ash adsorbent using after adopting microbial pretreatment to improve the rice husk surface nature, and this adsorbent is remarkable to grease pigment decolorizing effect, the rice husk commercial development is worth greatly improves.
The specific embodiment
Below in conjunction with specific embodiment, the present invention is described in further detail.Should be understood that these embodiment just in order to demonstrate the invention, but not limit the scope of the invention by any way.
Example 1: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is an aspergillus niger, the aspergillus niger nutrient solution is by adding cellulose powder 5g, potassium nitrate 30g, polyethylene glycol 1g in every premium on currency, pH6.5, inserting 50ml concentration is 10
7Cfu/ml aspergillus niger spore suspension, 32 ℃ of cultivation temperature, incubation time 130 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 50ml concentration is 10
7Cfu/ml whiterot fungi spore suspension, 25 ℃ of cultivation temperature were cultivated 210 hours.
In the 3rd step, the rice husk that ferments is dry handles 80 ℃ of baking temperatures, rice husk moisture content 8%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 120 ℃ of water smoking temperature, 30 minutes time; 260 ℃ of pre-charing phase temperature, 30 minutes time; 450 ℃ of charing phase temperature, 45 minutes time; 600 ℃ of calcination stage temperature, 90 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 2: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is an aspergillus niger, the aspergillus niger nutrient solution is by adding cellulose powder 5g, potassium nitrate 30g, polyethylene glycol 1g in every premium on currency, pH6.5, inserting 75ml concentration is 10
7Cfu/ml aspergillus niger spore suspension, 32 ℃ of cultivation temperature, incubation time 130 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 75ml concentration is 10
7Cfu/ml whiterot fungi spore suspension, 25 ℃ of cultivation temperature were cultivated 210 hours.
In the 3rd step, the rice husk that ferments is dry handles 80 ℃ of baking temperatures, rice husk moisture content 8%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 120 ℃ of water smoking temperature, 30 minutes time; 260 ℃ of pre-charing phase temperature, 30 minutes time; 450 ℃ of charing phase temperature, 45 minutes time; 600 ℃ of calcination stage temperature, 90 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 3: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is an aspergillus niger, the aspergillus niger nutrient solution is by adding cellulose powder 5g, potassium nitrate 30g, polyethylene glycol 1g in every premium on currency, pH6.5, inserting 100ml concentration is 10
7Cfu/ml aspergillus niger spore suspension, 32 ℃ of cultivation temperature, incubation time 130 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 100ml concentration is 10
7Cfu/ml whiterot fungi spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
In the 3rd step, the rice husk that ferments is dry handles 100 ℃ of baking temperatures, rice husk moisture content 12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 140 ℃ of water smoking temperature, 60 minutes time; 280 ℃ of pre-charing phase temperature, 60 minutes time; 500 ℃ of charing phase temperature, 75 minutes time; 650 ℃ of calcination stage temperature, 120 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 4: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is Trichoderma viride, koning trichoderma, and Trichoderma viride or koning trichoderma nutrient solution are by adding 2g (NH in every premium on currency
4)
2HPO
4, 0.0044g ZnSO
47H
2O, 0.2g K
2HPO
4, 0.001g MnSO
44H
2O, 0.8g KH
2PO
4, 0.005g FeSO
4, 0.9g MgSO
47H
2O, 0.005g Triammonium citrate, 2g peptone, 1g yeast extract, 0.001g/L V
B1, inserting 50ml concentration is 10
8Cfu/ml Trichoderma viride or koning trichoderma spore suspension, 28 ℃ of cultivation temperature were cultivated 96 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 100ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 28 ℃ of cultivation temperature were cultivated 250 hours.
In the 3rd step, the rice husk that ferments is dry handles 90 ℃ of baking temperatures, rice husk moisture content 10%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 130 ℃ of water smoking temperature, 45 minutes time; 270 ℃ of pre-charing phase temperature, 45 minutes time; 475 ℃ of charing phase temperature, 60 minutes time; 625 ℃ of calcination stage temperature, 105 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 5: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is Trichoderma viride, koning trichoderma, and Trichoderma viride or koning trichoderma nutrient solution are by adding 2g (NH in every premium on currency
4)
2HPO
4, 0.0044g ZnSO
47H
2O, 0.2g K
2HPO
4, 0.001g MnSO
44H
2O, 0.8g KH
2PO
4, 0.005g FeSO
4, 0.9g MgSO
47H
2O, 0.005g Triammonium citrate, 2g peptone, 1g yeast extract, 0.001g/L V
B1, inserting 75ml concentration is 10
8Cfu/ml Trichoderma viride or koning trichoderma spore suspension, 28 ℃ of cultivation temperature were cultivated 96 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 75ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 28 ℃ of cultivation temperature were cultivated 250 hours.
In the 3rd step, the rice husk that ferments is dry handles 90 ℃ of baking temperatures, rice husk moisture content 10%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 130 ℃ of water smoking temperature, 45 minutes time; 270 ℃ of pre-charing phase temperature, 45 minutes time; 475 ℃ of charing phase temperature, 60 minutes time; 625 ℃ of calcination stage temperature, 105 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 6: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is Trichoderma viride, koning trichoderma, and Trichoderma viride or koning trichoderma nutrient solution are by adding 2g (NH in every premium on currency
4)
2HPO
4, 0.0044g ZnSO
47H
2O, 0.2g K
2HPO
4, 0.001g MnSO
44H
2O, 0.8g KH
2PO
4, 0.005g FeSO
4, 0.9g MgSO
47H
2O, 0.005g Triammonium citrate, 2g peptone, 1g yeast extract, 0.001g/L V
B1, inserting 100ml concentration is 10
8Cfu/ml Trichoderma viride or koning trichoderma spore suspension, 28 ℃ of cultivation temperature were cultivated 96 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi, the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 100ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 28 ℃ of cultivation temperature were cultivated 250 hours.
In the 3rd step, the rice husk that ferments is dry handles 90 ℃ of baking temperatures, rice husk moisture content 10%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 130 ℃ of water smoking temperature, 45 minutes time; 270 ℃ of pre-charing phase temperature, 45 minutes time; 475 ℃ of charing phase temperature, 60 minutes time; 625 ℃ of calcination stage temperature, 105 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 7: produce rice hull ash adsorbent using according to following steps: the first step, to degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, the microorganism in the nutrient solution of cellulase-producing is a trichoderma reesei, the trichoderma reesei nutrient solution is by adding 10g (NH in every premium on currency
4)
2SO
4, 0.5g CaCl
2, 3g KH
2PO
4, 1g MgSO
47H
2O, inserting 50ml concentration is 10
8Cfu/ml trichoderma reesei spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 50 concentration is 10
7-10
8Cfu/ml whiterot fungi spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
In the 3rd step, the rice husk that ferments is dry handles 100 ℃ of baking temperatures, rice husk moisture content 12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 140 ℃ of water smoking temperature, 60 minutes time; 280 ℃ of pre-charing phase temperature, 60 minutes time; 500 ℃ of charing phase temperature, 75 minutes time; 650 ℃ of calcination stage temperature, 120 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 8: produce rice hull ash adsorbent using according to following steps: the first step, to degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, the microorganism in the nutrient solution of cellulase-producing is a trichoderma reesei, the trichoderma reesei nutrient solution is by adding 10g (NH in every premium on currency
4)
2SO
4, 0.5gCaCl
2, 3g KH
2PO
4, 1g MgSO
47H
2O, inserting 75ml concentration is 10
8Cfu/ml trichoderma reesei spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 75ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
In the 3rd step, the rice husk that ferments is dry handles 100 ℃ of baking temperatures, rice husk moisture content 12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 140 ℃ of water smoking temperature, 60 minutes time; 280 ℃ of pre-charing phase temperature, 60 minutes time; 500 ℃ of charing phase temperature, 75 minutes time; 650 ℃ of calcination stage temperature, 120 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 9: produce rice hull ash adsorbent using according to following steps: the first step, to degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, the microorganism in the nutrient solution of cellulase-producing is a trichoderma reesei, the trichoderma reesei nutrient solution is by adding 10g (NH in every premium on currency
4)
2SO
4, 0.5g CaCl
2, 3g KH
2PO
4, 1g MgSO
47H
2O, inserting 100ml concentration is 10
8Cfu/ml trichoderma reesei spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 100ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 30 ℃ of cultivation temperature were cultivated 300 hours.
In the 3rd step, the rice husk that ferments is dry handles 100 ℃ of baking temperatures, rice husk moisture content 12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 140 ℃ of water smoking temperature, 60 minutes time; 280 ℃ of pre-charing phase temperature, 60 minutes time; 500 ℃ of charing phase temperature, 75 minutes time; 650 ℃ of calcination stage temperature, 120 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 10: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is bacillus subtilis, bacillus licheniformis or bacillus cereus, and bacillus subtilis, bacillus licheniformis or bacillus cereus nutrient solution are by add 2g corn flour, 0.3g beef extract, 0.2g peptone, 0.5g NaCl, 0.1g KH in every premium on currency
2PO
4, 0.1g Na
2HPO
4, 0.05g MgSO
4, pH value 7.0, inserting 50ml concentration is 10
7Cfu/ml bacillus subtilis, bacillus licheniformis or bacillus cereus suspension, 37 ℃ of cultivation temperature were cultivated 56 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 50ml concentration is 10
7Cfu/ml whiterot fungi spore suspension, 25 ℃ of cultivation temperature were cultivated 210 hours.
In the 3rd step, the rice husk that ferments is dry handles 80 ℃ of baking temperatures, rice husk moisture content 8%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 120 ℃ of water smoking temperature, 30 minutes time; 260 ℃ of pre-charing phase temperature, 30 minutes time; 450 ℃ of charing phase temperature, 45 minutes time; 600 ℃ of calcination stage temperature, 90 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, rice hull ash gets adsorbent after the dry activation processing, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 11: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is bacillus subtilis, bacillus licheniformis or bacillus cereus, and bacillus subtilis, bacillus licheniformis or bacillus cereus nutrient solution are by add 2g corn flour, 0.3g beef extract, 0.2g peptone, 0.5g NaCl, 0.1g KH in every premium on currency
2PO
4, 0.1g Na
2HPO
4, 0.05g MgSO
4, pH value 7.0, inserting 75ml concentration is 10
8Cfu/ml bacillus subtilis, bacillus licheniformis or bacillus cereus suspension, 37 ℃ of cultivation temperature were cultivated 56 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 75ml concentration is 10
8Cfu/ml whiterot fungi spore suspension, 28 ℃ of cultivation temperature were cultivated 250 hours.
In the 3rd step, the rice husk that ferments is dry handles 90 ℃ of baking temperatures, rice husk moisture content 10%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 130 ℃ of water smoking temperature, 45 minutes time; 270 ℃ of pre-charing phase temperature, 45 minutes time; 475 ℃ of charing phase temperature, 60 minutes time; 625 ℃ of calcination stage temperature, 105 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Example 12: produce rice hull ash adsorbent using according to following steps: the first step, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, microorganism in the nutrient solution of cellulase-producing is bacillus subtilis, bacillus licheniformis or bacillus cereus, and bacillus subtilis, bacillus licheniformis or bacillus cereus nutrient solution are by add 2g corn flour, 0.3g beef extract, 0.2g peptone, 0.5g NaCl, 0.1g KH in every premium on currency
2PO
4, 0.1g Na
2HPO
4, 0.05g MgSO
4, pH value 7.0, inserting 100ml concentration is 10
7Cfu/ml bacillus subtilis, bacillus licheniformis or bacillus cereus suspension, 37 ℃ of cultivation temperature were cultivated 56 hours.
Second step, to ferment in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, the microorganism in the nutrient solution of product lignoenzyme is a whiterot fungi; The whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2gNa
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 100ml concentration is 10
7Cfu/ml whiterot fungi spore suspension, 28 ℃ of cultivation temperature were cultivated 250 hours.
In the 3rd step, the rice husk that ferments is dry handles 90 ℃ of baking temperatures, rice husk moisture content 10%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, 130 ℃ of water smoking temperature, 45 minutes time; 270 ℃ of pre-charing phase temperature, 45 minutes time; 475 ℃ of charing phase temperature, 60 minutes time; 625 ℃ of calcination stage temperature, 105 minutes time;
In the 5th step, the rice hull ash activation processing: per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, and 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, and adsorbent moisture is 8%.
Claims (7)
1. the method for preprocessing and producing rice hull ash adsorbent using with microbe, it is characterized in that: at first adopt two-step method that rice husk is carried out preliminary treatment, promptly improve the rice husk surface nature by cellulase-producing and lignoenzyme microorganism, rice hull ash is made in destructive distillation then, again to rice hull ash activate, dry rice hull ash adsorbent using.
2. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 1 is characterized in that comprising following concrete steps:
The first step, cellulase-producing microbial degradation rice husk, degrade in the nutrient solution of every liter of cellulase-producing of 20 gram rice husks addings, degradation time 50-130 hour, 25 ℃-37 ℃ of degradation temperatures, the microorganism in the nutrient solution of cellulase-producing are aspergillus niger, Trichoderma viride, koning trichoderma, trichoderma reesei, bacillus subtilis, bacillus licheniformis or wax sample bud bacillus;
Second goes on foot, and produces lignoenzyme microbial fermentation rice husk, ferments in the nutrient solution of every liter of product of 40 gram rice husks addings lignoenzyme, and fermentation time 210-300 hour, fermentation temperature 25-30 ℃, the microorganism in the nutrient solution of product lignoenzyme was a whiterot fungi;
In the 3rd step, the rice husk that ferments is dry to be handled, and baking temperature 80-100 ℃, rice husk moisture content 8-12%;
In the 4th step, rice husk destructive distillation stage by stage gets rice hull ash, and water smoking temperature 120-140 ℃, time 30-60 minute; 260-280 ℃ of pre-charing phase temperature, time 30-60 minute; 450-500 ℃ of charing phase temperature, time 45-75 minute; 600-650 ℃ of calcination stage temperature, time 90-120 minute;
The 5th step, the rice hull ash activation processing, per 30 gram rice hull ash are added 1 liter of activator activation, soak time 4h, 90 ℃ of activation temperatures, activation finishes the back ultra-clean and is washed to neutrality, and activator is 5% nitric acid and sulfuric acid by concentration and mixes at 1: 1 with volume ratio;
In the 6th step, the rice hull ash after the dry activation processing gets adsorbent, and at 4 hours rice hull ash adsorbent usings that get product of 150 ℃ of dryings of temperature, adsorbent moisture is 8%.
3. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 2 is characterized in that: the aspergillus niger nutrient solution is by adding cellulose powder 5g, potassium nitrate 30g, polyethylene glycol 1g in every premium on currency, inserting 50-100ml concentration is 10
7-10
8The aspergillus niger spore suspension of cfu/ml, pH6.5,32 ℃ of cultivation temperature, incubation time 130 hours.
4. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 2, it is characterized in that: Trichoderma viride, koning trichoderma nutrient solution are by adding 2g (NH in every premium on currency
4)
2HPO
4, 0.0044g ZnSO
47H
2O, 0.2g K
2HPO
4, 0.001g MnSO
44H
2O, 0.8gKH
2PO
4, 0.005g FeSO
4, 0.9g MgSO
47H
2O, 0.005g Triammonium citrate, 2g peptone, 1g yeast extract, 0.001g/L V
B1, inserting 50-100ml concentration is 10
7-10
8The Trichoderma viride of cfu/ml or koning trichoderma spore suspension, 28 ℃ of cultivation temperature were cultivated 96 hours.
5. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 2, it is characterized in that: the trichoderma reesei nutrient solution is by adding 10g (NH in every premium on currency
4)
2SO
4, 0.5gCaCl
2, 3g KH
2PO
4, 1g MgSO
47H
2O, inserting 50-100ml concentration is 10
7-10
8The trichoderma reesei spore suspension of cfu/ml, 28 ℃ of cultivation temperature were cultivated 96 hours.
6. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 2 is characterized in that: bacillus subtilis, bacillus licheniformis, bacillus cereus nutrient solution are by add 2g corn flour, 0.3g beef extract, 0.2g peptone, 0.5gNaCl, 0.1g KH in every premium on currency
2PO
4, 0.1g Na
2HPO
4, 0.05g MgSO
4, pH value 7.0, inserting 50-100ml concentration is 10
7-10
8The bacillus subtilis of cfu/ml, bacillus licheniformis or bacillus cereus suspension, 37 ℃ of cultivation temperature were cultivated 56 hours.
7. the method for preprocessing and producing rice hull ash adsorbent using with microbe according to claim 2 is characterized in that: the whiterot fungi nutrient solution is by adding 10g glucose, 0.1g ammonium tartrate, 0.5g MgSO in every premium on currency
47H
2O, 1.0g KH
2PO
4, 0.2g Na
2HPO
4, 0.035g MnSO
4, 0.007g CuSO
45H
2O, inserting 50-100ml concentration is 10
7-10
8The whiterot fungi spore suspension of cfu/ml, was cultivated 210-300 hour by cultivation temperature 25-30 ℃.
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