CN102978297B - Preparation method for high-concentration xylose hydrolysate - Google Patents
Preparation method for high-concentration xylose hydrolysate Download PDFInfo
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- CN102978297B CN102978297B CN201210544964.3A CN201210544964A CN102978297B CN 102978297 B CN102978297 B CN 102978297B CN 201210544964 A CN201210544964 A CN 201210544964A CN 102978297 B CN102978297 B CN 102978297B
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Abstract
The invention discloses a preparation method for high-concentration xylose hydrolysate, belonging to the technical field of production for functional sugars. According to the method, corncobs are treated by virtue of a sulphuric acid solution pre-soaking process before being hydrolyzed, xylose in the hydrolyzed corncobs is extracted by virtue of a countercurrent extraction process, materials and an extractant are moved along opposite directions in a leaching container, thus being continuously and adequately subjected to contact extraction; and a mode of positively charging materials and reversely inflowing water is adopted, the flowing of the materials and water is reversely continuous and dynamic flowing, so that the materials and water can keep relative motion, and active ingredients in the materials and the extractant always have a large concentration difference, so that the concentrations of the materials and the extractant diffuse and update to keep action, thus ensuring the fast extraction speed of the active ingredients and the high concentration of the extractant. The preparation method comprises the following process steps of: (1) pretreating, (2) soaking, (3) hydrolyzing, and (4) performing countercurrent extraction, wherein xylose in the hydrolyzed corncobs is extracted by virtue of a continuous countercurrent extraction device, so as to obtain the hydrolysate.
Description
Technical field
The utility model belongs to technical field of functional sugar production, is specifically related to a kind of agriculture that utilizes corn cob, bagasse, bamboo bits etc. to be rich in pentosan, forestry waste and prepares the method for high density xylose hydrolysis fluid for raw material.
Background technology
Wood sugar is a kind of five-carbon sugar, molecular formula C
5h
10o
5, be present in the form of pentosan in agriculture, the forestry waste such as corn cob, bagasse, bamboo bits.Wood sugar is to produce the main raw material of Xylitol, because of Xylitol have low in calories, take in and do not improve blood glucose value, can improve the function affects such as liver function, preventing dental caries and fat-reducing and be widely used in diabetics's sweeting agent, nutritious supplementary and auxiliary therapeutical agent and sugar-free or food with low sugar content.
At present, the preparation method who extracts wood sugar from agriculture, the forestry waste such as corn cob, bagasse, bamboo bits is mainly sulphuric acid hydrolysis, and sulfuric acid is catalyzer.
The main technique method of sulphuric acid hydrolysis is: the raw materials such as corn cob, after pre-treatment, add 1.2% sulfuric acid under 120 DEG C of conditions, to be incubated hydrolysis 150 minutes by solid-to-liquid ratio 1:8, then utilizes the filtration unit in hydrolytic decomposition pot to separate hydrolyzed solution and hydrolysis residue.In order to extract the wood sugar in corn cob completely, need to be again to the deionized water that adds 4 times of volumes of corn cob quality in hydrolytic decomposition pot after hydrolysis discharge opeing, 100 DEG C are incubated 30 minutes, discharge opeing obtains secondary hydrolyzed solution, after mixing with primary hydrolyzed solution, obtain mixed hydrolysis liquid, hydrolyzed solution concentration is generally at 6-8%; And then respectively adding at twice the deionized water of 4 times of volumes to wash, washing water are used for allocating sulphuric acid soln.Not only complex operation of whole hydrolysis process, the production cycle is also very long, completes whole requirements of process 12-15 hour.
Can from corn cob, wood sugar be extracted completely although do like this, but due to will be through twice hydrolysis, twice washing, thus the problems such as the large and concentrated steam consumption of hydrolyzed solution of hydrolyzing process exists complicated operation, the production cycle is long, plant factor is low, water consumption is large, hydrolyzed solution concentration is low and caused greatly by water consumption hydrolysis temperature-rise period steam consumption is large caused.
Hydrolyzing process is the first operation of xylose production, is to be related to the quality of finished product wood sugar and the key of postorder operation tooling cost.How to solve the problem existing in current hydrolysis process and directly have influence on the development of following wood sugar industry.
Summary of the invention
The object of this invention is to provide a kind of preparation method of high density xylose hydrolysis fluid, to solve prior art hydrolysis process complicated operation, the problem such as the production cycle is long, and plant factor is low, and water consumption is large, and hydrolyzed solution concentration is on the low side, and steam consumption is large.
The technique that the technical solution adopted for the present invention to solve the technical problems adopts corn cob to soak in advance with sulphuric acid soln before hydrolysis and the wood sugar utilizing in the rear corn cob of countercurrent extraction technique extraction hydrolysis, allow the rear corn cob of hydrolysis and extraction agent move in opposite directions in extraction vessel, contact continuously and fully extraction; Adopt forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water, make material and water can keep relative movement, and in material there is a larger concentration difference in effective constituent and extraction agent all the time, make feed concentration diffusion upgrade continuous action, and then ensured that extracts active ingredients speed is fast and extract concentration is high.Its preparation method processing step is as follows:
1, pre-treatment
Utilize screen scarifier dust removal soil, foreign material in small, broken bits, adopt rotary drum washer water machine, dust, foreign material, pigment on raw material corn cob are washed, forefinger is shown in true qualities, no-sundries.
2, soak
By the complete submergence of concentration 0.5-2.0% sulphuric acid soln for pretreated corn cob.Soak time 2-8 hour.20 DEG C-100 DEG C of soaking temperatures.Sulphuric acid soln soakage is 1.5-3 times of corn cob weight.
3, hydrolysis
The corn cob soaking with sulphuric acid soln is drained to surface solution, at 105-130 DEG C of temperature, be hydrolyzed 90-180 minute.Utilizing sulfuric acid that corn cob sucks in immersion process to make catalyzer is hydrolyzed and obtains monomolecular wood sugar pentosan.
4, countercurrent extraction
Corn cob after hydrolysis utilizes continuous counter-flow extraction equipment to extract wood sugar wherein, obtains hydrolyzed solution.Hydrolyzed solution concentration 12-18%.Concrete operations mode is: the corn cob after hydrolysis is sent into continuous counter-flow extraction equipment by opening for feed, the deionized water that corn cob is 20-80 DEG C with the temperature that passes into from fluid inlet under the promotion of spiral propeller forms inverse motion, and the corn cob of processing is in discharge port discharge and spent acid solution is discharged from leakage fluid dram.The ratio of the fltting speed of corn cob and the fltting speed of water is 0.3-0.8(m
3/ m
3).
Adopting positively effect of the present invention is to utilize sulphuric acid soln immersion treatment corn cob can reduce the consumption of water consumption and catalyst sulfuric acid, and the wood sugar that utilizes continuous countercurrent extraction process to extract in corn cob also can reduce water consumption and improve hydrolyzed solution concentration.Totally can realize and improve hydrolyzed solution concentration 1-2 doubly, reduce sulfuric acid consumption 50%, reduce water consumption approximately 60%, steam consumption approximately 60%, shortens hydrolysis time more than 6 hours, has improved the utilization ratio of equipment, can significantly reduce the production cost of wood sugar, estimate per tonly to reduce costs 3000 yuan.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
1, pre-treatment
Utilize screen scarifier dust removal soil, foreign material in small, broken bits, adopt rotary drum washer water machine, dust, foreign material, pigment on raw material corn cob are washed, forefinger is shown in true qualities, no-sundries.
2, soak
By the complete submergence of concentration 1.0% sulphuric acid soln for pretreated corn cob.Soak time 5 hours.25 DEG C of soaking temperatures.Sulphuric acid soln soakage is 2.5 times of corn cob weight.
3, hydrolysis
The corn cob soaking with sulphuric acid soln is drained to surface solution, at 115 DEG C of temperature, be hydrolyzed 120 minutes.
4, countercurrent extraction
Corn cob after hydrolysis is sent into continuous counter-flow extraction equipment by opening for feed, the deionized water that corn cob is 30 DEG C with the temperature passing into from fluid inlet under the promotion of spiral propeller forms inverse motion, the corn cob of processing discharge port discharge and spent acid solution is discharged from leakage fluid dram, obtain hydrolyzed solution, the ratio of the fltting speed of corn cob and the fltting speed of water is 0.4(m
3/ m
3).Hydrolyzed solution concentration 15%.
Embodiment 2
1, pre-treatment
Utilize screen scarifier dust removal soil, foreign material in small, broken bits, adopt rotary drum washer water machine, dust, foreign material, pigment on raw material corn cob are washed, forefinger is shown in true qualities, no-sundries.
2, soak
By the complete submergence of concentration 1.0% sulphuric acid soln for pretreated corn cob.Soak time 5 hours.50 DEG C of soaking temperatures.Sulphuric acid soln soakage is 2.6 times of corn cob weight.
3, hydrolysis
The corn cob soaking with sulphuric acid soln is drained to surface solution, at 120 DEG C of temperature, be hydrolyzed 150 minutes.
4, countercurrent extraction
Corn cob after hydrolysis is sent into continuous counter-flow extraction equipment by opening for feed, the deionized water that corn cob is 30 DEG C with the temperature passing into from fluid inlet under the promotion of spiral propeller forms inverse motion, the corn cob of processing discharge port discharge and spent acid solution is discharged from leakage fluid dram, obtain hydrolyzed solution, the ratio of the fltting speed of corn cob and the fltting speed of water is 0.6(m
3/ m
3).Hydrolyzed solution concentration 12%.
Claims (1)
1. the preparation method of a high density xylose hydrolysis fluid, it is characterized in that before being hydrolyzed by corn cob with sulphuric acid soln soaking technology and utilize countercurrent extraction technique to extract the wood sugar in corn cob after hydrolysis in advance, allow material and extraction agent move in opposite directions in leaching container, contact continuously and fully extraction; Adopt forward feeding, oppositely water inlet, flowing for reverse continuous dynamic flow of material and water, make material and water can keep relative movement, and in material there is a larger concentration difference in effective constituent and extraction agent all the time, make feed concentration diffusion upgrade continuous action, and then ensured that extracts active ingredients speed is fast and extract concentration is high; Its preparation method processing step is as follows:
(1) pre-treatment: utilize screen scarifier dust removal soil, foreign material in small, broken bits, adopt rotary drum washer water machine, dust, foreign material, pigment on raw material corn cob are washed, forefinger is shown in true qualities, no-sundries;
(2) soak: by the complete submergence of pretreated corn cob concentration 0.5-2.0% sulphuric acid soln; Soak time 2-8 hour; 20 DEG C-100 DEG C of soaking temperatures; Sulphuric acid soln soakage is 1.5-3 times of corn cob weight;
(3) hydrolysis: the corn cob soaking with sulphuric acid soln is drained to surface solution, be hydrolyzed 90-180 minute at 105-130 DEG C of temperature; Utilizing sulfuric acid that corn cob sucks in immersion process to make catalyzer is hydrolyzed and obtains monomolecular wood sugar pentosan;
(4) countercurrent extraction: the corn cob after hydrolysis utilizes continuous counter-flow extraction equipment to extract wood sugar wherein, obtains hydrolyzed solution; Hydrolyzed solution concentration 12-18%; Concrete operations mode is: the corn cob after hydrolysis is sent into continuous counter-flow extraction equipment by opening for feed, the deionized water that corn cob is 20-80 DEG C with the temperature that passes into from fluid inlet under the promotion of spiral propeller forms inverse motion, and the corn cob of processing is in discharge port discharge and spent acid solution is discharged from leakage fluid dram; The ratio of the fltting speed of corn cob and the fltting speed of water is 0.3-0.8(m
3/ m
3).
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