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CN1107447C - 仓储熏蒸杀虫剂磷化镁的合成工艺 - Google Patents

仓储熏蒸杀虫剂磷化镁的合成工艺 Download PDF

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Publication number
CN1107447C
CN1107447C CN99112883A CN99112883A CN1107447C CN 1107447 C CN1107447 C CN 1107447C CN 99112883 A CN99112883 A CN 99112883A CN 99112883 A CN99112883 A CN 99112883A CN 1107447 C CN1107447 C CN 1107447C
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CN
China
Prior art keywords
fumigating insecticide
red phosphorus
reaction
magnesium
magnesium phosphide
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Expired - Fee Related
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CN99112883A
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CN1271524A (zh
Inventor
杜继德
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shenyang harvest pesticide Co., Ltd.
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HUAREN (SHENYANG) AGRICULTURAL CHEMICALS CO Ltd
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Priority to CN99112883A priority Critical patent/CN1107447C/zh
Publication of CN1271524A publication Critical patent/CN1271524A/zh
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Abstract

仓储熏蒸杀虫剂磷化镁的合成工艺，是采用镁粉、赤磷为原料，在有减缓反应速度的添加剂如C18-25的脂肪酸或其盐、C24-26的氯代烷烃、碱土金属氧化物、碳酸盐，其中之一或几种存在下，用电热引发反应制得。该熏蒸杀虫剂用手仓储粮食熏蒸杀虫，尤其用于船运货物的熏蒸杀虫。

Description

仓储熏蒸杀虫剂磷化镁的合成工艺
本发明属于农用仓储熏蒸杀虫剂。
磷化镁作为仓储熏蒸杀虫剂比磷化铝易分解，由于分解速度快，缩短了熏蒸时间，取得了较好的药效，扩大了应用面。可用于气温较低的仓储条件下熏蒸杀虫及特殊需要的仓储熏蒸杀虫，尤其是大型船运货物的熏蒸杀虫，缩短了船泊停港时间，大大降低滞港费用。
U.S，4331642、U.S，4,412.979-专利报道，目前德国迪盖公司已有磷化镁生产，但该公司采用的工艺路线为黄磷法，即在通惰性气体氩气的条件下在带有搅拌的密闭反应器中，在催化剂引发下不断加入镁粉及黄磷进行反应合成磷化镁，该过程需要设有加热、冷却、物料输送、氩气保护等设施。该方法流程长、能耗大，氩气保护提高了成本。为克服上述的不足，本发明提出用镁粉、赤磷，在有减缓反应速度的添加剂存在下，在尽量排出空气的密闭式反应器中，用电热引发反应，即镁热法制得磷化镁。该工艺省掉了加热、冷却、物料运输、氩气保护等设施，因此有流程短、设备少、能耗小、生产投资低等优点。
本发明的具体实施方案
1、选定原料镁粉的规格为：
活性镁含量＞94％；
粒度40-80纲目全通过。
2、在配料中加入总原料量的2-15％添加剂。添加剂采用C18-25的脂肪酸或其盐、C24-26氯代烷烃,碱土金属氧化物、碳酸盐，其中之一或几种。
3、本发明提供的镁热法工艺及半密闭式反应器是根据镁粉与赤磷反应是不可逆放热反应，反应一旦引发，便自动进行下去。为实现镁热法工艺，设计了半密闭式反应器，避免了反应物料与空气接触产生剧烈反应及喷料，又避免反应过程中赤磷受热氧化，使反应器内气体膨胀时造成内压剧增。
实例1将符合质量要求的镁粉与赤磷按1∶0.28-0.86(重量)比，以及原料总量的2-15％的C24氯代烷烃作为添加剂进行充分混合后，装入反应器中，电热引发反应，待反应物料温度隆至100℃以下，即可出料，可得产品磷化镁，收率以镁粉计＞95％，含量＞90％。

Claims (2)

1、仓储熏蒸杀虫剂磷化镁的合成工艺，其特征在于采用镁粉、赤磷为原料，加入减缓反应速度的添加剂，在排出空气的密闭式反应器中，电热引发反应制得磷化镁，反应中所用的添加剂为C24-26的氯代烷烃。
2、根据权利要求1所述的合成工艺，其特征在于所用原料镁粉、赤磷的用量比为1∶0.28-0.86(重量比)，减缓反应速度所用的添加剂的量为镁粉和赤磷总重量的2-15％。
CN99112883A 1999-04-27 1999-04-27 仓储熏蒸杀虫剂磷化镁的合成工艺 Expired - Fee Related CN1107447C (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN99112883A CN1107447C (zh) 1999-04-27 1999-04-27 仓储熏蒸杀虫剂磷化镁的合成工艺

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN99112883A CN1107447C (zh) 1999-04-27 1999-04-27 仓储熏蒸杀虫剂磷化镁的合成工艺

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CN1271524A CN1271524A (zh) 2000-11-01
CN1107447C true CN1107447C (zh) 2003-05-07

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Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102351158B (zh) * 2011-07-14 2013-02-13 马文忠 利用黄磷生产磷化铝同时回收副产品的工艺方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3532464A (en) * 1966-04-07 1970-10-06 Werner Freyberg Method of making magnesium phosphide
EP0028315A1 (de) * 1979-10-31 1981-05-13 Hoechst Aktiengesellschaft Verfahren zur Herstellung von Magnesiumphosphid
US4331642A (en) * 1979-11-12 1982-05-25 Degesch Gmbh Process for preparing aluminum or magnesium phosphide
GB2097775A (en) * 1981-05-02 1982-11-10 Deutsche Ges Schaedlingsbek Production of aluminium or magnesium phosphide
JPH09278618A (ja) * 1996-04-04 1997-10-28 Eiichi Kagaku Kogyo Kk リン化水素生成殺虫剤の製造方法

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3532464A (en) * 1966-04-07 1970-10-06 Werner Freyberg Method of making magnesium phosphide
EP0028315A1 (de) * 1979-10-31 1981-05-13 Hoechst Aktiengesellschaft Verfahren zur Herstellung von Magnesiumphosphid
US4331642A (en) * 1979-11-12 1982-05-25 Degesch Gmbh Process for preparing aluminum or magnesium phosphide
GB2097775A (en) * 1981-05-02 1982-11-10 Deutsche Ges Schaedlingsbek Production of aluminium or magnesium phosphide
JPH09278618A (ja) * 1996-04-04 1997-10-28 Eiichi Kagaku Kogyo Kk リン化水素生成殺虫剤の製造方法

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Owner name: SHENYANG FENGSHOU PESTICIDE CO., LTD.

Free format text: FORMER OWNER: HUAREN (SHENYANG) AGRICULTURAL CHEMICALS CO., LTD.

Effective date: 20040924

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Address after: 110108, No. 100, Ji Dong Road, Lin Sheng Town, Sujiatun District, Liaoning, Shenyang

Patentee after: Shenyang harvest pesticide Co., Ltd.

Address before: 110101 No. 101 Haitang street, Sujiatun District, Liaoning, Shenyang

Patentee before: Huaren (Shenyang) Agricultural Chemicals Co., Ltd.

C19 Lapse of patent right due to non-payment of the annual fee
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