Regular　Mn-Zn-Mg-Al-CO　3　quaternary　layered　double　hydroxides(LDHs)　were　synthesized　by　hydrothermal　method　in　one　step,　using　Mn(NO　3)　2·6H　2O,　Zn(NO　3)　2·6H　2O,　Mg(NO　3)　2·6H　2O　and　Al(N0　3)　3·9H　2O　as　raw　materials.　ICP,　Elemental　Analysis,　XRD,　IR,　TG-DSC,　SEM,　low　temperature　nitrogen　adsorption-desorption　were　used　to　characterize　the　composition,　crystallinity,　structure,　morphology　and　performance　of　the　obtained　materials.　The　effects　of　pH　value,　reaction　temperature,　reaction　time,　molar　ratio　of　raw　materials　on　the　structure　of　Mn-Zn-Mg-Al-CO　3　quaternary　LDHs　were　investigated.　The　results　show　that　Mn-Zn-Mg-Al-CO　3　quaternary　LDHs　with　well-defined　shape,　obvious　intercalated　structure　and　well　regular　quality　could　be　obtained　at　pH　value　about　10,　the　hydrothermal　temperature　of　140　°C　and　reaction　time　of　24　h.　The　nitrogen　adsorption-desorption　results　suggest　that　the　isothermal　type　of　the　sample　is　type　V,　hysteresis　loop　resembls　the　H3-type　in　the　IUPAC　classification.　The　samples　have　highly　ordered　intimate　structure,　neatly　arranged　interlayer　anions,　high　hole　density,　small　aperture　and　large　surface　area.