CN104352532B - A kind of fermentation cordyceps purifying technique - Google Patents
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- 241000190633 Cordyceps Species 0.000 title claims abstract description 43
- 238000000855 fermentation Methods 0.000 title claims abstract description 12
- 230000004151 fermentation Effects 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 title claims abstract description 11
- 239000000706 filtrate Substances 0.000 claims abstract description 28
- 239000003513 alkali Substances 0.000 claims abstract description 25
- 238000000108 ultra-filtration Methods 0.000 claims abstract description 24
- 239000007787 solid Substances 0.000 claims abstract description 21
- 238000004140 cleaning Methods 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000005554 pickling Methods 0.000 claims abstract description 9
- 238000003801 milling Methods 0.000 claims abstract description 5
- 238000005374 membrane filtration Methods 0.000 claims abstract description 3
- 239000012528 membrane Substances 0.000 claims description 57
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 47
- 238000001471 micro-filtration Methods 0.000 claims description 32
- 239000000843 powder Substances 0.000 claims description 29
- 239000000243 solution Substances 0.000 claims description 29
- 238000005406 washing Methods 0.000 claims description 27
- 239000007788 liquid Substances 0.000 claims description 24
- 239000002253 acid Substances 0.000 claims description 21
- 239000000919 ceramic Substances 0.000 claims description 10
- 239000011148 porous material Substances 0.000 claims description 8
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 239000012141 concentrate Substances 0.000 claims description 6
- 241001248610 Ophiocordyceps sinensis Species 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910017604 nitric acid Inorganic materials 0.000 claims description 3
- 241000894006 Bacteria Species 0.000 claims 3
- 235000021110 pickles Nutrition 0.000 claims 2
- 238000001816 cooling Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 claims 1
- 239000012530 fluid Substances 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 238000004064 recycling Methods 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 2
- 238000000227 grinding Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 238000012545 processing Methods 0.000 abstract description 2
- 238000007873 sieving Methods 0.000 abstract description 2
- 238000000746 purification Methods 0.000 description 9
- 238000011084 recovery Methods 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 4
- 239000008399 tap water Substances 0.000 description 4
- 235000020679 tap water Nutrition 0.000 description 4
- 230000007613 environmental effect Effects 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 239000012467 final product Substances 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- A61K36/062—Ascomycota
- A61K36/066—Clavicipitaceae
- A61K36/068—Cordyceps
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Abstract
Description
技术领域technical field
本发明涉及发酵虫草菌粉制备工艺，特别是一种发酵虫草菌粉提纯工艺。The invention relates to a preparation process of fermented Cordyceps powder, in particular to a purification process of fermented Cordyceps powder.
背景技术Background technique
冬虫夏草是海拔3000米至5000米的高原特有产物，市场供应量有限，需要大量的替代品，而人工发酵的虫草菌粉则是主要的替代品之一。尽管虫草菌粉发酵量大，但是其提取工艺陈旧，目前主要是采用板框过滤的方式来使发酵液固液分离，这种分离方式耗能大，板框布安装和拆卸困难，需要大量人工操作，不易自动化，处理量有限，维护保养较难，且其滤液含有大量颗粒较大的物质，既降低收率，又对环境造成污染，增加环保压力。常用的板框工艺中虫草菌粉的固形物收率75％左右。因此，需要发明更适合现代低碳环保要求的发酵虫草菌粉提纯工艺。Cordyceps sinensis is a unique product of the plateau at an altitude of 3,000 to 5,000 meters. The market supply is limited and a large number of substitutes are needed, and artificially fermented Cordyceps fungus powder is one of the main substitutes. Although the fermentation capacity of Cordyceps fungus powder is large, its extraction process is outdated. At present, the method of plate and frame filtration is mainly used to separate the solid and liquid of the fermentation liquid. This separation method consumes a lot of energy, and the installation and disassembly of the plate and frame cloth is difficult, requiring a lot of labor. The operation is not easy to automate, the processing capacity is limited, and the maintenance is difficult, and the filtrate contains a large number of substances with large particles, which not only reduces the yield, but also pollutes the environment and increases the pressure on environmental protection. The solid yield of Cordyceps powder in the commonly used plate and frame process is about 75%. Therefore, it is necessary to invent a purification process for fermented Cordyceps powder that is more suitable for modern low-carbon environmental protection requirements.
发明内容Contents of the invention
本发明提出一种发酵虫草菌粉提纯工艺，具有环保无二次污染的特点，制备的成品中发酵虫草菌粉固形物收率高于98％，解决了现有技术生产的发酵虫草菌粉固形物收率低且易造成环境污染的缺点。The invention proposes a purification process of fermented Cordyceps powder, which has the characteristics of environmental protection and no secondary pollution. The solid yield of fermented Cordyceps powder in the prepared finished product is higher than 98%. The disadvantages of low yield and easy to cause environmental pollution.
本发明的技术方案是这样实现的：Technical scheme of the present invention is realized like this:
一种发酵虫草菌粉提纯工艺，其包括如下步骤：A process for purifying fermented Cordyceps powder, comprising the steps of:
S1、清洗步骤：S1. Cleaning steps:
S11、用自来水清洗微滤膜和超滤膜，直至清洗液澄清，之后用碱液洗涤，控制碱液的温度、浓度和碱洗时间，洗涤结束后得到碱洗微滤膜和碱洗超滤膜；收集碱洗液至碱液收集罐中；S11, clean the microfiltration membrane and the ultrafiltration membrane with tap water until the cleaning solution is clear, then wash with lye, control the temperature, concentration and alkali washing time of the lye, and obtain the alkali-washed microfiltration membrane and alkali-washed ultrafiltration after washing Membrane; collect the alkali washing liquid into the alkali liquid collection tank;
S12、将S11得到的碱洗微滤膜和碱洗超滤膜用自来水洗涤，直至洗涤液呈中性，用酸液洗涤，控制酸液的浓度和洗涤时间，检测酸液通过微滤膜的流速，当流速高于设定值时，停止酸洗；用纯净水继续洗涤，直至洗涤液呈中性，得到干净的微滤膜和干净的超滤膜；收集酸洗液至酸液收集罐中；S12, washing the alkali-washed microfiltration membrane and the alkali-washed ultrafiltration membrane obtained in S11 with tap water until the washing solution is neutral, washing with acid solution, controlling the concentration and washing time of the acid solution, and detecting the acid solution passing through the microfiltration membrane. Flow rate, when the flow rate is higher than the set value, stop pickling; continue washing with pure water until the washing liquid is neutral, and get a clean microfiltration membrane and a clean ultrafiltration membrane; collect the pickling liquid to the acid liquid collection tank middle;
S2、过滤步骤：S2, filtering step:
S21、将发酵虫草菌粉液引入微滤膜缓冲罐中，经S12中干净的微滤膜过滤，检测滤液流速，收集滤液至超滤膜缓冲罐中，当滤液流速低于设定的微滤膜流速时，停止过滤，将发酵虫草菌粉微滤浓缩液收集至干燥罐中；S21. Introduce the fermented Cordyceps powder into the microfiltration membrane buffer tank, filter through the clean microfiltration membrane in S12, detect the flow rate of the filtrate, collect the filtrate into the ultrafiltration membrane buffer tank, when the filtrate flow rate is lower than the set microfiltration When the membrane flow rate is high, the filtration is stopped, and the microfiltration concentrate of the fermented Cordyceps powder is collected into a drying tank;
S22、将S21中超滤膜缓冲罐中的滤液经S12中干净的超滤膜过滤，收集滤液至回收罐中，停止过滤后将发酵虫草菌粉超滤浓缩液收集至干燥罐中；S22. Filtrate the filtrate in the ultrafiltration membrane buffer tank in S21 through the clean ultrafiltration membrane in S12, collect the filtrate into the recovery tank, and collect the fermented Cordyceps powder ultrafiltration concentrate in the drying tank after stopping the filtration;
S23、将S22中收集的滤液加入S12中收集的酸洗液，得到酸滤液，混合10小时后再加入S11中收集的碱洗液进行中和，检测合格后排放；S23, adding the filtrate collected in S22 to the pickling liquid collected in S12 to obtain the acid filtrate, after mixing for 10 hours, add the alkali washing liquid collected in S11 for neutralization, and discharge after passing the test;
S3、干燥步骤：S3, drying step:
将S21和S22得到的干燥罐中浓缩液烘干，检测固体中的水分含量，当水分含量低于设定的水分值时，停止烘干，冷却得到发酵虫草菌固体；Dry the concentrated liquid in the drying tank obtained in S21 and S22, detect the moisture content in the solid, stop drying when the moisture content is lower than the set moisture value, and cool to obtain the fermented Cordyceps solid;
S4、制粉步骤：S4, milling step:
将S3得到的发酵虫草菌固体研磨，用标准筛过筛后得到发酵虫草菌粉体。Grinding the fermented Cordyceps solid obtained in S3, and sieving with a standard sieve to obtain fermented Cordyceps powder.
进一步的，S11中碱液为NaOH和NaClO组成的混合溶液，其中NaOH的浓度为1-2wt％，NaClO的浓度为0.5-1wt％，碱液的温度为60-70℃，碱洗时间为20-30min。Further, the lye in S11 is a mixed solution composed of NaOH and NaClO, wherein the concentration of NaOH is 1-2wt%, the concentration of NaClO is 0.5-1wt%, the temperature of the lye is 60-70°C, and the alkali washing time is 20 -30min.
进一步的，S12中酸液为HNO3溶液，HNO3的浓度为0.5-1.5wt％，酸液流速设定值为360L/h/m2。Further, the acid solution in S12 is HNO 3 solution, the concentration of HNO 3 is 0.5-1.5 wt%, and the acid solution flow rate is set at 360L/h/m 2 .
进一步的，S21中的微滤膜是过滤孔径为的陶瓷膜450-600nm，S22中的超滤膜是过滤孔径为150-300nm的陶瓷膜。Further, the microfiltration membrane in S21 is a ceramic membrane with a filtration pore diameter of 450-600 nm, and the ultrafiltration membrane in S22 is a ceramic membrane with a filtration pore diameter of 150-300 nm.
进一步的，S21中设定的微滤膜流速为65L/(h·m2)。Further, the flow rate of the microfiltration membrane set in S21 is 65 L/(h·m 2 ).
进一步的，S3中设定的水分值为3wt％。Further, the moisture value set in S3 is 3wt%.
进一步的，S4中标准筛的目数为100目。Further, the mesh number of the standard sieve in S4 is 100 mesh.
相对现有技术，本发明具有以下优点：Compared with the prior art, the present invention has the following advantages:
(1)本发明提出的发酵虫草菌粉提纯工艺，依次经清洗步骤、过滤步骤、干燥步骤和制粉步骤，得到最终产品，最终产品中发酵虫草菌粉固形物收率高于98％。(1) The purification process of the fermented Cordyceps powder proposed by the present invention, through the cleaning step, the filtering step, the drying step and the milling step, obtains the final product in sequence, and the solid yield of the fermented Cordyceps powder in the final product is higher than 98%.
(2)本发明提出的发酵虫草菌粉提纯工艺中收集的酸洗液用于氧化滤液中的有机物等，碱洗液与酸滤液中和后排放，最终排放液达到工业排放标准，无二次污染。(2) The pickling liquid collected in the purification process of the fermented Cordyceps powder proposed by the present invention is used to oxidize the organic matter in the filtrate, etc., and the alkaline washing liquid and the acid filtrate are neutralized and discharged, and the final discharge liquid reaches the industrial discharge standard without secondary pollute.
附图说明Description of drawings
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例或现有技术描述中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings that need to be used in the description of the embodiments or the prior art. Obviously, the accompanying drawings in the following description are only These are some embodiments of the present invention. Those skilled in the art can also obtain other drawings based on these drawings without creative work.
图1是本发明发酵虫草菌粉提纯工艺的工艺流程图。Fig. 1 is the process flow diagram of the purification process of fermented Cordyceps powder of the present invention.
具体实施方式detailed description
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
参照图1，一种发酵虫草菌粉提纯工艺，以100kg固含量为26.7wt％的发酵虫草菌粉液为原料进行提纯，选用过滤孔径为600nm的陶瓷膜作为微滤膜，选用过滤孔径为300nm的陶瓷膜作为超滤膜，提纯工艺包括如下步骤：With reference to Fig. 1, a kind of fermented Cordyceps powder purification process, with 100kg solid content is the fermented Cordyceps powder liquid of 26.7wt% to carry out purification as raw material, selects the ceramic membrane that filter aperture is 600nm as microfiltration membrane, selects filter aperture to be 300nm The ceramic membrane is used as an ultrafiltration membrane, and the purification process includes the following steps:
S1、清洗步骤：S1. Cleaning steps:
S11、用自来水清洗微滤膜和超滤膜，直至清洗液澄清，之后用碱液洗涤，碱液为NaOH和NaClO组成的混合溶液，其中NaOH的浓度为1wt％，NaClO的浓度为0.5wt％，控制碱液的温度为60℃，碱洗时间为30min，洗涤结束后得到碱洗微滤膜和碱洗超滤膜；收集碱洗液至碱液收集罐中；S11, clean the microfiltration membrane and ultrafiltration membrane with tap water until the cleaning solution is clear, then wash with lye, the lye is a mixed solution of NaOH and NaClO, wherein the concentration of NaOH is 1wt%, and the concentration of NaClO is 0.5wt% , controlling the temperature of the lye to be 60°C, and the alkali washing time to be 30 minutes, to obtain an alkali-washed microfiltration membrane and an alkali-cleaned ultrafiltration membrane after washing; collect the alkali wash solution into the alkali solution collection tank;
S12、将S11得到的碱洗微滤膜和碱洗超滤膜用自来水洗涤，直至洗涤液呈中性，用酸液洗涤，酸液为HNO3溶液，HNO3的浓度为0.5wt％，控制酸液的浓度和洗涤时间，检测酸液通过微滤膜的流速，当流速高于设360L/(h·m2)，停止酸洗；用纯净水继续洗涤，直至洗涤液呈中性，得到干净的微滤膜和干净的超滤膜；收集酸洗液至酸液收集罐中；S12, washing the alkali-washed microfiltration membrane and the alkali-washed ultrafiltration membrane obtained in S11 with tap water until the washing liquid is neutral, and washing with an acid solution, the acid solution is HNO solution, and the concentration of HNO is 0.5wt%. The concentration of the acid solution and the washing time are used to detect the flow rate of the acid solution through the microfiltration membrane. When the flow rate is higher than the set 360L/(h·m 2 ), the pickling is stopped; the washing is continued with pure water until the washing solution is neutral, and the obtained Clean microfiltration membrane and clean ultrafiltration membrane; collect pickling liquid into acid liquid collection tank;
S2、过滤步骤：S2, filtering step:
S21、将发酵虫草菌粉液引入微滤膜缓冲罐中，经S12中干净的微滤膜过滤，检测滤液流速，收集滤液至超滤膜缓冲罐中，当滤液流速低于65L/(h·m2)，停止过滤，将发酵虫草菌粉微滤浓缩液收集至干燥罐中；S21, introduce the fermented Cordyceps powder into the microfiltration membrane buffer tank, filter through the clean microfiltration membrane in S12, detect the filtrate flow rate, collect the filtrate in the ultrafiltration membrane buffer tank, when the filtrate flow rate is lower than 65L/(h· m 2 ), stop filtering, and collect the fermented Cordyceps powder microfiltration concentrate in a drying tank;
S22、将S21中超滤膜缓冲罐中的滤液经S12中干净的超滤膜过滤，收集滤液至回收罐中，停止过滤后将发酵虫草菌粉超滤浓缩液收集至干燥罐中；S22. Filtrate the filtrate in the ultrafiltration membrane buffer tank in S21 through the clean ultrafiltration membrane in S12, collect the filtrate into the recovery tank, and collect the fermented Cordyceps powder ultrafiltration concentrate in the drying tank after stopping the filtration;
S23、将S22中收集的滤液加入S12中收集的酸洗液，得到酸滤液，混合10小时后再加入S11中收集的碱洗液进行中和，检测合格后排放；S23, adding the filtrate collected in S22 to the pickling liquid collected in S12 to obtain the acid filtrate, after mixing for 10 hours, add the alkali washing liquid collected in S11 for neutralization, and discharge after passing the test;
S3、干燥步骤：S3, drying step:
将S21和S22得到的干燥罐中浓缩液烘干，检测固体中的水分含量，当水分含量低于3wt％时，停止烘干，冷却得到发酵虫草菌固体；Dry the concentrated liquid in the drying tank obtained in S21 and S22, detect the moisture content in the solid, stop drying when the moisture content is lower than 3wt%, and cool to obtain the fermented Cordyceps solid;
S4、制粉步骤：S4, milling step:
将S3得到的发酵虫草菌固体研磨，用100目的标准筛过筛后得到发酵虫草菌粉体。Grind the fermented Cordyceps solid obtained in S3, and sieve through a 100-mesh standard sieve to obtain fermented Cordyceps powder.
最终得到发酵虫草菌粉体26.22kg，固体回收率为98.2％。Finally, 26.22 kg of fermented Cordyceps powder was obtained, and the solid recovery rate was 98.2%.
实施例2Example 2
本实施例与实施1基本相同，不同之处在于：This embodiment is basically the same as Implementation 1, the difference is:
以100kg固含量为31.2％的发酵虫草菌粉液进行提纯；Purify with 100kg of fermented Cordyceps powder with a solid content of 31.2%;
S11中NaOH的浓度为1.5wt％，NaClO的浓度为0.7wt％，碱液的温度为605℃，碱洗时间为25min。The concentration of NaOH in S11 is 1.5wt%, the concentration of NaClO is 0.7wt%, the temperature of the lye is 605°C, and the alkali washing time is 25min.
S12中HNO3的浓度为1wt％。The concentration of HNO3 in S12 was 1 wt%.
S21中的微滤膜是过滤孔径为500nm的陶瓷膜，S22中的超滤膜是过滤孔径为200nm的陶瓷膜。The microfiltration membrane in S21 is a ceramic membrane with a filter pore size of 500nm, and the ultrafiltration membrane in S22 is a ceramic membrane with a filter pore size of 200nm.
最终得到发酵虫草菌粉体30.76kg，固体回收率为98.6％。Finally, 30.76 kg of fermented Cordyceps powder was obtained, and the solid recovery rate was 98.6%.
实施例3Example 3
本实施例与实施例1基本相同，不同之处在于：This embodiment is basically the same as Embodiment 1, the difference is:
以100kg固含量为34.5％的发酵虫草菌粉液进行提纯；Purify with 100kg of fermented Cordyceps powder with a solid content of 34.5%;
S11NaOH的浓度为2wt％，NaClO的浓度为1wt％，碱液的温度为70℃，碱洗时间为20min。The concentration of S11NaOH is 2wt%, the concentration of NaClO is 1wt%, the temperature of the lye is 70°C, and the alkali washing time is 20min.
S12中HNO3的浓度为1.5wt％。The concentration of HNO3 in S12 was 1.5 wt%.
S21中的微滤膜是过滤孔径为450nm的陶瓷膜，S22中的超滤膜是过滤孔径为150nm的陶瓷膜。The microfiltration membrane in S21 is a ceramic membrane with a filter pore size of 450nm, and the ultrafiltration membrane in S22 is a ceramic membrane with a filter pore size of 150nm.
最终得到发酵虫草菌粉体34.12kg，固体回收率为98.9％。Finally, 34.12 kg of fermented Cordyceps powder was obtained, and the solid recovery rate was 98.9%.
以上所述仅为本发明的较佳实施例而已，并不用以限制本发明，凡在本发明的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本发明的保护范围之内。The above descriptions are only preferred embodiments of the present invention, and are not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included in the scope of the present invention. within the scope of protection.
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| CN103214533A (en) * | 2013-04-19 | 2013-07-24 | 湖南农业大学 | Method for continuously preparing cordycepin and cordyceps polysaccharide by using membrane separation technology |
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