CN114208823A - 一种可分散油悬浮剂用精炼矿物油的制备方法及应用 - Google Patents
一种可分散油悬浮剂用精炼矿物油的制备方法及应用 Download PDFInfo
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- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
- A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N61/00—Biocides, pest repellants or attractants, or plant growth regulators containing substances of unknown or undetermined composition, e.g. substances characterised only by the mode of action
- A01N61/02—Mineral oils; Tar oils; Tar; Distillates, extracts or conversion products thereof
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G67/00—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only
- C10G67/02—Treatment of hydrocarbon oils by at least one hydrotreatment process and at least one process for refining in the absence of hydrogen only plural serial stages only
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/205—Metal content
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2400/00—Products obtained by processes covered by groups C10G9/00 - C10G69/14
- C10G2400/18—Solvents
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Abstract
本发明公开了一种可分散油悬浮剂用精炼矿物油的制备方法及应用。本发明以10号工业白油经过加氢精制工艺,得到可用于可分散油悬浮剂的精炼矿物油,该精炼矿物油的质量指标及理化指标均满足可分散油悬浮剂开发特点和国家对农用精炼矿物油的要求。本发明的精炼矿物油非常适用于可分散油悬浮剂,在农业使用时可避免药害的同时,发挥最佳药效,具有很高的安全性。
Description
技术领域
本发明属于农化技术领域,具体涉及一种可分散油悬浮剂用精炼矿物油的制备及应用。
背景技术
纵观农药发展史,随着环保意识的提高及可持续发展的需要,对农药剂型的要求越来越高,农药行业亟待开发和优化新型农药剂型,可分散油悬浮剂具有环保、高效的特点,近些年日益受到行业研究者的关注和重视。
可分散油悬浮剂(Oil Dispersion,简称OD)是指一种或一种以上在非水分散介质(主要包括油基介质或溶剂介质)中不溶的农药固体活性成分,通过研磨加工成微细颗粒,再依靠某些助剂均匀地分散于非水分散介质中,形成的一种高分散、高悬浮、能流动的稳定液体制剂。
可分散性油悬浮剂的配方包括原药、表面活性剂、粘度调节剂、分散剂、稳定剂、分散介质等多个组分。其中,分散介质作为原药的分散和稀释载体,是可分散性油悬浮剂中占比最大的组分,它对可分散油悬浮剂产品的性能影响很大,主要表现在对农药活性成分含量的热稳定性、制剂稳定性、使用的安全性、药效等方面。因此,分散介质的选择要考虑两方面,一是要足够稳定,既不能使农药活性成分分解发生反应,也不能溶解,要求溶解度越小越好,这样才能确保产品的稳定和安全;二是要有增效作用,用作分散介质的非水介质要具有良好的铺展性和粘附性,可以增加药液在靶标上的沉积量和持留时间,提高药效。
油类具有一定粘度,用于可分散油悬浮剂产品增效明显,常用的油类分散介质有植物油类(如大豆油),矿物油类(如白油)和油酸甲酯(如菜籽油甲基酯、大豆油甲基酯、棕榈甲酯油等)。
其中,油酸甲酯是目前市场上常用的分散介质,其主要优点是药效快,靶向性较好,但缺点也明显,油酸甲酯极性较大,不同厂家的产品差异明显,有的因工艺问题带入少量极性更强的醇类杂质、或者碳链分布范围太广、对配方影响较大,极性过大也会导致在高温时易加剧一些除草剂的药害。低温时制剂不易生产,有些助剂对不同原药相同的油酸甲酯并不是能通用。同样的,植物油类极性更大,粘度可选择性也少,用于开发成可分散油悬浮剂的原药产品少,如大豆油的粘度比较高,只适合选择做低含量的制剂配方,且大豆油相对不易乳化,易起泡。
目前油酸甲酯或植物油在可分散油悬浮剂配方开发过程中,均存在体系不稳定,有效成分分解率高,贮存稳定性差的现象,例如对于非常适用于开发成可分散油悬浮剂剂型的除草剂烟嘧磺隆,这些问题尤为明显。
鉴于此,有必要提供一种可分散油悬浮剂用的精炼矿物油,以解决可分散油悬浮剂分散介质的选择和质量问题。
发明内容
本发明涉及一种可分散油悬浮剂用精炼矿物油的制备方法及应用,具体涉及一种精炼矿物油,该发明的精炼矿物油极性化合物含量极低,对组分结构和碳数分布等质量指标进行限制,与原药相互作用小,物理化学性质稳定,非常适用于开发可分散油悬浮剂,在农业使用时可避免药害的同时,发挥最佳药效,具有很高的安全性。
本发明采用的技术方案如下
一种可分散油悬浮剂用精炼矿物油的制备方法包括:
选用10号工业白油经过加氢精制,得到可用于可分散油悬浮剂用精炼矿物油。
所述的可分散油悬浮剂用精炼矿物油的加氢精制过程为:10号工业白油经换热后进入至温度(320℃)的炉加热,与循环氢混合。油料混合物进入反应器,通过催化剂(Ni-Mo或Ni-W型)床层进行加氢反应,加氢生成油交换和冷却后依次进入高、低压分离,从低压分离器分出的加氢生成油经过加热,然后送入分馏塔,把残留在油中的气体和轻馏分汽提出去,由塔底出来的生成油经过热换冷却后即为精炼矿物油。其中,催化加氢反应过程中:10号工业白油与循环氢形成的油料混合物在反应器的催化剂床层上进行加氢反应,该过程将10号工业白油中硫、氧、氮等杂质转换成硫化氢、水、氨而除去,并使烯烃和芳烃等不饱和烃类加氢饱和,大大降低所得产物的总芳烃+极性化合物含量、硫含量,提升非磺化物含量。汽提过程中:加氢生成油交换和冷却后依次进入高、低压分离器,从低压分离器分出的加氢生成油经过加热,送入分馏塔,把残留在油中的气体和轻馏分汽提出去,由塔底出来的生成油经过热换冷却后即为精炼矿物油。该过程通过高、低压分离器和分馏塔,将加氢生成油的高馏分段和低馏分段组分切割去除,使所得产物的馏程范围减小,最终得到理想碳数分布的精炼矿物油。
本发明的可分散油悬浮剂用精炼矿物油的控制指标:总芳烃+极性化合物含量≤1%,10%相对正构烷烃碳数≥19,90%相对正构烷烃碳数≤24,相对正构烷烃碳数范围差≤5,相对正构烷烃平均碳数21-22,非磺化物含量≥99.5%,链烷烃含量≥70,分子量290~310。
本发明的可分散油悬浮剂用精炼矿物油,其理化性质指标的参数:无色无味,40℃运动粘度为9.50-10.50mm2/s,20℃密度≤825.0kg/m3,开口闪点≥150℃,倾点≤-20℃。
本发明的可分散油悬浮剂用精炼矿物油,其硫、水分及重金属含量指标的参数为:硫含量≤10mg/kg,水分≤50mg/kg,铅(Pb)≤10mg/kg,砷(As)≤10mg/kg,重金属≤20mg/kg。
与均为极性或弱极性化合物的油酸甲酯和植物油相比,本发明采用特殊处理的精炼矿物油作为分散介质用于可分散油悬浮剂的制备,其中矿物油为非极性饱和烷烃的混合物,能够稳定分散绝大多数极性原药,与大多数极性原药不会发生反应或溶解,而且上游石油炼化企业的原料非常丰富,通过加氢精制等工艺处理精炼矿物油,组分结构和碳数范围可控,不易起泡,凝固点低,较低温度依然能保持流动,此外,精炼矿物油自身具有杀虫、杀菌作用。因此,以精炼矿物油开发的可分散油悬浮剂,性质稳定,理化指标好,粘附性和展着性优异,能明显提高农药的防治效果,降低农药的使用量。
具体实施方式
下面结合实施例对本发明作进一步说明,但本发明不限于下述实施例。
实施例1:
以石化公司提供的10号工业白油为原料,经换热后进入至温度(240~350℃)的炉加热,与循环氢混合。油料混合物进入反应器,设置压力在10-30MPa,反应温度为150-300℃,空速为0.1-0.6(体积)/h,氢油比为600-800(体积),通过催化剂(Ni-Mo型)床层进行加氢反应,加氢生成油交换和冷却后依次进入高、低压分离,设置高压在20~30MPa,低压8~20Mpa,从低压分离器分出的加氢生成油经过加热,温度控制150~300℃,然后送入分馏塔,把残留在油中的气体和轻馏分汽提出去,由塔底出来的生成油经过热换冷却后即为精炼矿物油。
表1为本发明可分散油悬浮剂用精炼矿物油指标参数及测定方法。
实施例2:
以精炼矿物油分散介质的40g/L烟嘧磺隆OD除草剂的开发。
为了提高用于农药的矿物油产品质量,2008年中华人民共和国农业部发布了第1133号公告,该公告规定了生产矿物油农药的质量指标,主要包括相对正构烷烃碳数差、相对正构烷烃平均碳数范围和非磺化物含量等3个质量指标,本实施例选用满足农业部第1133号公告要求的实施例1中精炼矿物油。
以重量百分比计量,4%烟嘧磺隆、14%表面活性剂、1.5%稳定剂、80.5%精炼矿物油分散介质。所述的表面活性剂为蓖麻油聚氧乙烯醚系列、(C9~C11直链)脂肪醇聚氧乙烯和司盘系列、吐温系列,所述稳定剂为1:1的有机膨润土和白炭黑,分散介质为实施例1中精炼矿物油。
按照国标GB 28155-2011烟嘧磺隆可分散油悬浮剂评价标准,对以本发明的精炼矿物油制备的40g/L烟嘧磺隆OD与市售产品进行对比,市售产品为以油酸甲酯制备的40g/L烟嘧磺隆OD(对比例1)和以大豆油制备的40g/L烟嘧磺隆OD(对比例2)产品进行对比评价,结果为表2。
由表2可以看出,采用实施例1精炼矿物油制备的40g/L烟嘧磺隆OD产品质量指标远远超过国家标准的要求,与市售的以油酸甲酯制备的40g/L烟嘧磺隆OD和以大豆油制备的40g/L烟嘧磺隆OD产品相比,分解率得到有效控制,有效提高了烟嚰磺隆可分散油悬浮剂的储存时间,稳定性更好。
实施例3:
以精炼矿物油分散介质的100g/L烟嘧磺隆OD除草剂的开发。
本实施例选用满足农业部第1133号公告要求的实施例1中精炼矿物油。以重量百分比计量,10%烟嘧磺隆、12%表面活性剂、3%稳定剂、75%精炼矿物油分散介质。所述的表面活性剂为蓖麻油聚氧乙烯醚系列、(C9~C11直链)脂肪醇聚氧乙烯和司盘系列、吐温系列,所述稳定剂为1:1的有机膨润土和白炭黑,分散介质为实施例1中精炼矿物油。
按照国标GB 28155-2011烟嘧磺隆可分散油悬浮剂评价标准,对以本发明的精炼矿物油制备的100g/L烟嘧磺隆OD与市售的产品进行对比,市售产品为以油酸甲酯制备的100g/L烟嘧磺隆OD(对比例3)和以大豆油制备的100g/L烟嘧磺隆OD(对比例4)产品进行对比评价,结果为表3。
由表3可以看出,采用实施例1精炼矿物油制备的100g/L烟嘧磺隆OD产品质量指标远远超过国家标准的要求,与市售的以油酸甲酯制备的100g/L烟嘧磺隆OD和以大豆油制备的100g/L烟嘧磺隆OD产品相比,分解率得到有效控制,有效提高了烟嚰磺隆可分散油悬浮剂的储存时间,稳定性更好。
Claims (6)
1.一种可分散油悬浮剂用精炼矿物油的制备方法,其特征在于,包括如下:
选用10号工业白油经过加氢精制,得到可分散油悬浮剂用精炼矿物油。
2.根据权利要求1所述的可分散油悬浮剂用精炼矿物油的制备方法,其特征在于,所述的加氢精制过程为:
将10号工业白油经换热后进入至320℃的炉中加热,与循环氢混合,油料混合物进入反应器,通过催化剂床层进行加氢反应,所述催化剂为Ni-Mo或Ni-W型,加氢生成油交换和冷却后依次进入高、低压分离器,从低压分离器分出的加氢生成油经过加热,送入分馏塔,把残留在油中的气体和轻馏分汽提出去,由塔底出来的生成油经过热换冷却后即为精炼矿物油。
3.根据权利要求1所述的可分散油悬浮剂用精炼矿物油的制备方法,其特征在于,可分散油悬浮剂用精炼矿物油的控制指标为:总芳烃+极性化合物含量≤1%,10%相对正构烷烃碳数≥19,90%相对正构烷烃碳数≤24,相对正构烷烃碳数范围差≤5,相对正构烷烃平均碳数21-22,非磺化物含量≥99.5%,链烷烃含量≥70,分子量290~310。
4.根据权利要求1所述的可分散油悬浮剂用精炼矿物油的制备方法,其特征在于,所述精炼矿物油,其理化性质指标的参数为:无色无味,40℃运动粘度为9.50-10.50mm2/s,20℃密度≤825.0kg/m3,开口闪点≥150℃,倾点≤-20℃。
5.根据权利要求1所述的可分散油悬浮剂用精炼矿物油的制备方法,其特征在于,所述精炼矿物油,其硫、水分及重金属含量指标的参数为:硫含量≤10mg/kg,水分≤50mg/kg,铅(Pb)≤10mg/kg,砷(As)≤10mg/kg,重金属≤20mg/kg。
6.一种农药,其特征在于,以权利要求1-5任一项所述方法制得的精炼矿物油作为分散介质制得。
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