CN105900984A - 一种生物质水热碳化液相制备农药、固相制备有机肥的方法 - Google Patents

一种生物质水热碳化液相制备农药、固相制备有机肥的方法 Download PDF

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CN105900984A
CN105900984A CN201610264525.5A CN201610264525A CN105900984A CN 105900984 A CN105900984 A CN 105900984A CN 201610264525 A CN201610264525 A CN 201610264525A CN 105900984 A CN105900984 A CN 105900984A
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付严
官懿
余永龙
叶振文
张飞宏
肖阳
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South China University of Technology SCUT
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Abstract

本发明属于生物质资源利用技术领域，公开了一种生物质水热碳化液相制备农药、固相制备有机肥的方法。所述方法为：将生物质原料与水混合均匀得到生物质水溶液，然后将其加入到高压反应器中，用惰性气体或氢气置换反应器内空气，升温至200～300℃，搅拌条件下进行恒温水热碳化反应，反应产物经过滤或离心分离，液相经乙酸乙酯萃取后制备农药，固相干燥后制备有机肥。与传统的生物油水相组分糖及糖类衍生物制备农药及有机肥方法相比，该方法具有能耗低、反应条件温和、工艺过程简单、反应产物易分离、对环境友好等优点。

Description

一种生物质水热碳化液相制备农药、固相制备有机肥的方法
技术领域
本发明属于生物质资源利用技术领域，具体涉及一种生物质水热碳化液相制备农药、固相制备有机肥的方法。
背景技术
柑橘渣、蔗渣是食品工业的废弃物，价格低廉具有数量大、产地集中，其成分单一不需要分选处理、质量可控等优势。与其他类型的农林生物质资源比较，柑橘渣、蔗渣是很好的生物质炼制工业的原料。本发明开发一种新的利用工艺，采用水热碳化的方法，不用催化剂，制备肥料及农药，既保护了环境，又实现了生物质废弃物还田，增加了土壤的肥力，还克服了直接还田柑橘渣、蔗渣中木质素不易腐烂的缺点。具有重要的现实意义。有广泛的市场前景。
传统的控释肥料是农林废弃物经过粉碎、提取、过滤、浓缩、发酵、造粒、烘干、冷却、包裹等步骤制成的。生物质中的木质素是无法腐烂的，一般采用田头焚烧办法处理，造成了空气污染。
发明内容
为了解决以上现有技术的缺点和不足之处，本发明的首要目的在于提供一种生物质水热碳化液相制备农药、固相制备有机肥的方法。
本发明的另一目的在于提供一种通过上述方法制备得到的农药和有机肥。
本发明目的通过以下技术方案实现：
一种生物质水热碳化液相制备农药、固相制备有机肥的方法，所述方法包括以下制备步骤：
将生物质原料与水混合均匀得到生物质水溶液，然后将其加入到高压反应器中，用惰性气体或氢气置换反应器内空气，升温至200～300℃，搅拌条件下进行恒温水热碳化反应，反应产物经过滤或离心分离，液相经乙酸乙酯萃取后制备农药，固相干燥后制备有机肥。上述水热碳化反应产物的分离流程图如图1所示。
所述的生物质原料优选蔗渣或柑橘渣。
所述生物质水溶液中生物质原料的质量浓度优选为6％～10％。
所述生物质水溶液的体积优选为高压反应器体积的1/3～3/4。
所述搅拌的速度优选为100～1000转/分钟。
所述水热碳化反应的时间优选为4～24h。
一种农药和有机肥，通过上述方法制备得到。
本发明的原理为：生物质水溶液在高温条件下产生生物油组分，其中富含糖(如：左旋葡聚糖)及糖的衍生物(如：低分子量醛、5-羟甲基糠醛、羟乙醛、羟丙酮等)。本发明利用糖类及其衍生物易聚合特性，通过水热碳化方法在高压反应釜中，200℃～300℃恒温条件，将水相糖类及其衍生物聚合，并进一步碳化，过滤分离得到有机肥。同时，通过简单分离萃取获得富含酚类的液相组分用以生产农药。
本发明具有如下优点及有益效果：
(1)本发明采用水热碳化方法，液相产物富含杀菌力很强的糠醛以及苯酚及其衍生物，稀释后可作为农药使用，固相有机碳继承了生物质中大部分营养成分，可作为肥料施用；
(2)本发明解决了生物油体系中因糖类及其衍生物存在造成的生物油体系不稳定性问题；将其中不稳定的因素糖类及其衍生物通过聚合碳化并用简单分离方法制备有机肥；同时通过萃取分离获得了富含酚类等稳定组分的水相产物可用于制备农药；该方法反应原料及过程低毒、过程简单、能耗低、反应条件温和；
(3)采用本发明提供的生物质水溶液制备有机肥及农药，可以一边热解，一边分离，原料处理简单，设备技术灵活及经济性好，能够实现生产过程的连续化，适合工业化应用。
附图说明
图1是本发明水热碳化反应产物的分离流程图；
图2是实施例2水热碳化后液体产物乙酸乙酯萃取GC-MS总离子流谱图。
具体实施方式
下面结合实施例及附图对本发明作进一步详细的描述，但本发明的实施方式不限于此。
实施例1
将蔗渣3g与水50mL混合均匀得到生物质水溶液，然后将其加入到150mL高压反应器中，盖紧釜盖，用氮气对反应釜中空气进行置换4次。然后，打开反应釜冷凝装置及电源，设定反应温度225℃，搅拌速度800转/分钟。升温至225℃后，恒温5小时。反应终止，取出反应釜冷却至常温，放气，打开釜盖。取出反应所产生的固体焦炭及富含酚类等稳定组分的水相产物，用布氏漏斗进行分离，固体烘干获得有机肥，液相产物经乙酸乙酯萃取后用于制备农药。
实施例2
将蔗渣3g与水50mL混合均匀得到生物质水溶液，然后将其加入到150mL高压反应器中，盖紧釜盖，用氮气对反应釜中空气进行置换4次。然后，打开反应釜冷凝装置及电源，设定反应温度255℃，搅拌速度800转/分钟。升温至255℃后，恒温5小时。反应终止，取出反应釜冷却至常温，放气，打开釜盖。取出反应所产生的固体焦炭及富含酚类等稳定组分的水相产物，用布氏漏斗进行分离，固体烘干获得有机肥，液相产物经乙酸乙酯萃取后用于制备农药。
实施例3
将蔗渣3g与水50mL混合均匀得到生物质水溶液，然后将其加入到150mL高压反应器中，盖紧釜盖，用氮气对反应釜中空气进行置换4次。然后，打开反应釜冷凝装置及电源，设定反应温度265℃，搅拌速度800转/分钟。升温至265℃后，恒温5小时。反应终止，取出反应釜冷却至常温，放气，打开釜盖。取出反应所产生的固体焦炭及富含酚类等稳定组分的水相产物，用布氏漏斗进行分离，固体烘干获得有机肥，液相产物经乙酸乙酯萃取后用于制备农药。
实施例4
将柑橘渣5g与水50mL混合均匀得到生物质水溶液，然后将其加入到150mL高压反应器中，盖紧釜盖，用氮气对反应釜中空气进行置换4次。然后，打开反应釜冷凝装置及电源，设定反应温度290℃，搅拌速度800转/分钟。升温至290℃后，恒温24小时。反应终止，取出反应釜冷却至常温，放气，打开釜盖。取出反应所产生的固体焦炭及富含酚类等稳定组分的水相产物，用布氏漏斗进行分离，固体烘干获得有机肥，液相产物经乙酸乙酯萃取后用于制备农药。
实施例1～3所得固相产率及液相产率结果如表1所示：
表1
序号 压力/Mpa 液相质量 固体质量 总质量 液相产率 固相产率
实施例1 1.996 2.02g 0.89g 2.91g 67.33％ 29.67％
实施例2 2.012 2.22g 0.67g 2.89g 74％ 22.33％
实施例3 2.018 2.31g 0.58g 2.89g 77％ 19.33％
实施例2水热碳化后液体产物经乙酸乙酯萃取后GC-MS总离子流谱图如图2所示，其产物主要组分及相对含量如表2所示：
表2
上述实施例为本发明较佳的实施方式，但本发明的实施方式并不受上述实施例的限制，其它的任何未背离本发明的精神实质与原理下所作的改变、修饰、替代、组合、简化，均应为等效的置换方式，都包含在本发明的保护范围之内。

Claims (7)

1.一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于所述方法包括以下制备步骤：
将生物质原料与水混合均匀得到生物质水溶液，然后将其加入到高压反应器中，用惰性气体或氢气置换反应器内空气，升温至200～300℃，搅拌条件下进行恒温水热碳化反应，反应产物经过滤或离心分离，液相经乙酸乙酯萃取后制备农药，固相干燥后制备有机肥。
2.根据权利要求1所述的一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于：所述的生物质原料是指蔗渣或柑橘渣。
3.根据权利要求1所述的一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于：所述生物质水溶液中生物质原料的质量浓度为6％～10％。
4.根据权利要求1所述的一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于：所述生物质水溶液的体积为高压反应器体积的1/3～3/4。
5.根据权利要求1所述的一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于：所述搅拌的速度为100～1000转/分钟。
6.根据权利要求1所述的一种生物质水热碳化液相制备农药、固相制备有机肥的方法，其特征在于：所述水热碳化反应的时间为4～24h。
7.一种农药和有机肥，其特征在于：通过权利要求1～6任一项所述的方法制备得到。
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